CN112741866A - Processing preparation process and detection method for pinellia ternata producing area - Google Patents
Processing preparation process and detection method for pinellia ternata producing area Download PDFInfo
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- 241001522232 Pinellia ternata Species 0.000 title claims abstract description 110
- 238000012545 processing Methods 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000001514 detection method Methods 0.000 title claims abstract description 22
- 241001522129 Pinellia Species 0.000 claims abstract description 195
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 130
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 86
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 86
- 239000004571 lime Substances 0.000 claims abstract description 86
- 238000000034 method Methods 0.000 claims abstract description 67
- 150000007524 organic acids Chemical class 0.000 claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 56
- 229930013930 alkaloid Natural products 0.000 claims abstract description 37
- 238000002791 soaking Methods 0.000 claims abstract description 29
- 230000008569 process Effects 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 219
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 153
- 238000005303 weighing Methods 0.000 claims description 128
- 239000003814 drug Substances 0.000 claims description 100
- 239000000843 powder Substances 0.000 claims description 76
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 72
- 238000001035 drying Methods 0.000 claims description 70
- 239000000243 solution Substances 0.000 claims description 66
- 238000001816 cooling Methods 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- 238000000605 extraction Methods 0.000 claims description 36
- 238000001914 filtration Methods 0.000 claims description 34
- 229940079593 drug Drugs 0.000 claims description 31
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 27
- 239000000523 sample Substances 0.000 claims description 27
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- 239000000047 product Substances 0.000 claims description 21
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- 238000004448 titration Methods 0.000 claims description 17
- 239000000706 filtrate Substances 0.000 claims description 13
- 239000012488 sample solution Substances 0.000 claims description 12
- 238000002835 absorbance Methods 0.000 claims description 11
- ZPLCXHWYPWVJDL-UHFFFAOYSA-N 4-[(4-hydroxyphenyl)methyl]-1,3-oxazolidin-2-one Chemical compound C1=CC(O)=CC=C1CC1NC(=O)OC1 ZPLCXHWYPWVJDL-UHFFFAOYSA-N 0.000 claims description 10
- 238000007865 diluting Methods 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 239000007853 buffer solution Substances 0.000 claims description 9
- 239000012086 standard solution Substances 0.000 claims description 9
- 239000012085 test solution Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 238000009736 wetting Methods 0.000 claims description 5
- 150000003797 alkaloid derivatives Chemical class 0.000 abstract description 27
- 238000000643 oven drying Methods 0.000 abstract description 13
- 238000000855 fermentation Methods 0.000 abstract description 8
- 230000004151 fermentation Effects 0.000 abstract description 8
- 238000003672 processing method Methods 0.000 abstract description 8
- 238000011160 research Methods 0.000 abstract description 6
- 238000011156 evaluation Methods 0.000 abstract description 5
- 235000005985 organic acids Nutrition 0.000 abstract description 4
- 229960001701 chloroform Drugs 0.000 description 97
- 238000005516 engineering process Methods 0.000 description 24
- 235000019441 ethanol Nutrition 0.000 description 23
- 238000012360 testing method Methods 0.000 description 23
- 238000003756 stirring Methods 0.000 description 17
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- 238000002156 mixing Methods 0.000 description 14
- 238000004458 analytical method Methods 0.000 description 10
- 238000011835 investigation Methods 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 7
- BALXUFOVQVENIU-GNAZCLTHSA-N Ephedrine hydrochloride Chemical compound Cl.CN[C@@H](C)[C@H](O)C1=CC=CC=C1 BALXUFOVQVENIU-GNAZCLTHSA-N 0.000 description 6
- 229960002534 ephedrine hydrochloride Drugs 0.000 description 6
- 206010062717 Increased upper airway secretion Diseases 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 208000026435 phlegm Diseases 0.000 description 5
- 230000004580 weight loss Effects 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 235000021107 fermented food Nutrition 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 230000000149 penetrating effect Effects 0.000 description 4
- 239000013558 reference substance Substances 0.000 description 4
- 238000013077 scoring method Methods 0.000 description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 3
- 238000000540 analysis of variance Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 229940093915 gynecological organic acid Drugs 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 206010011224 Cough Diseases 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 206010047700 Vomiting Diseases 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 235000003704 aspartic acid Nutrition 0.000 description 2
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 2
- 229940001584 sodium metabisulfite Drugs 0.000 description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 210000001519 tissue Anatomy 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- HLLSOEKIMZEGFV-UHFFFAOYSA-N 4-(dibutylsulfamoyl)benzoic acid Chemical compound CCCCN(CCCC)S(=O)(=O)C1=CC=C(C(O)=O)C=C1 HLLSOEKIMZEGFV-UHFFFAOYSA-N 0.000 description 1
- 206010000060 Abdominal distension Diseases 0.000 description 1
- 241000209524 Araceae Species 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 206010067171 Regurgitation Diseases 0.000 description 1
- 208000013738 Sleep Initiation and Maintenance disease Diseases 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 206010000269 abscess Diseases 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000020965 cold beverage Nutrition 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002790 cross-validation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003665 fog water Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000000819 hypertonic solution Substances 0.000 description 1
- 229940021223 hypertonic solution Drugs 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 206010022437 insomnia Diseases 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 230000024121 nodulation Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000012088 reference solution Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 206010042772 syncope Diseases 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/888—Araceae (Arum family), e.g. caladium, calla lily or skunk cabbage
- A61K36/8888—Pinellia
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
- G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/13—Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Molecular Biology (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a processing and preparation process and a detection method of pinellia ternate producing areas, wherein the research takes total organic acid and total alkaloid as detection indexes, and comprehensive evaluation is carried out through experimental results to obtain the processing method of pinellia ternate, which comprises the following steps: grading rhizoma Pinelliae according to 0.5cm difference, soaking in 5 wt% lime or lime water, peeling, and oven drying at 35 deg.C. The method has the advantages of simple and easy process, easy peeling in the fermentation process, low breakage rate, white color and fresh color of the finished product, and high content of total alkaloids and total organic acids, and is stable, reasonable and feasible, and provides high value for guiding the production of pinellia ternata medicinal materials.
Description
Technical Field
The invention relates to the field of traditional Chinese medicine processing, in particular to a processing preparation process and a detection method for pinellia ternate producing areas.
Background
Pinellia ternata is a plant of Araceae, is a clinically common traditional Chinese medicine, and is pungent, warm in nature and toxic; it enters spleen, stomach and lung meridians. The main effects and functions are as follows: dry dampness and resolve phlegm, check adverse rise of qi and stop vomiting, relieve stuffiness and dissipate nodulation; treating damp phlegm cold drink, emesis, regurgitation, cough, asthma, excessive phlegm, fullness and distention of chest and diaphragm, phlegm syncope, headache, dizziness and insomnia; abscess and swelling in the exterior.
At present, common steps of a processing method of fresh pinellia ternata comprise fermentation, peeling and drying.
(1) Fermentation: the harvested fresh tuber of pinellia is directly stacked in a stacking chamber for 15-20 days, and the fermentation method has the technical problems that the tuber of pinellia is easy to discolor, the fermentation is not uniform, the peeling effect is influenced and the like. (2) Peeling: at present, the peeling mode comprises mechanical peeling and manual peeling. Mechanical peeling is to screen the fermented tuber of pinellia tuber into three stages, namely large, medium and small, put the pinellia tuber of the same grade into a peeling machine and turn over the tuber continuously to peel. Manually peeling, most of the pinellia tuber after fermentation is respectively put into woven bags or other containers, after water washing, the pinellia tuber is put through rubber boots and treaded or repeatedly rubbed by hands, then the pinellia tuber is poured into a sieve to be rinsed with water to remove broken skin, and the cocoon tuber without clean skin is picked out and rubbed again until all the pinellia tuber is cleaned. (3) And (3) drying: the method comprises the common methods of airing, insolating, drying and the like, wherein the airing and the insolating need to be continuously insolated in a sunning ground with sufficient sunshine and good ventilation condition, and the influence of anti-fog water is greatly influenced by external conditions; the pinellia ternate is easy to be affected by external conditions, sticky, fermented and even rotten due to long drying time, and the pinellia ternate is usually treated by a sulfur smoking method or directly mixed with sodium metabisulfite chemicals to ensure that the surface of the pinellia ternate is white and has the functions of killing insects and preventing corrosion in order to facilitate storage. However, sulfur or sodium metabisulfite can generate chemical components such as sulfur dioxide in the processing process, easily penetrate cell walls to be attached to starch granules, penetrate into the tissue of the medicinal material and react with certain components in the tissue of the medicinal material, and further influence the quality of the medicinal material.
Application number CN201110147028.4, a pinellia ternate and a processing method thereof, discloses the following steps: peeling fresh rhizoma Pinelliae, cleaning, soaking in acidic solution with pH of 1-6 for 2-30min, taking out, washing residual acidic solution on surface, and drying.
The technical problem of application No. CN201110147028.4 is: acid soaking causes pinellia ternate to contain acidic residues, and the quality of the pinellia ternate is influenced; the long acid soaking time can cause the chemical reaction of the traditional Chinese medicine components of the pinellia ternata and the acid, reduce the effective components of the pinellia ternata and influence the quality; the processing method is easy to corrode processing equipment and high in cost.
The invention discloses a processing method of a fresh pinellia tuber producing area with application number CN201710798222.6, which fully utilizes the physiological characteristics of pinellia tuber plant cells, reduces the content of calcium oxalate crystals which is a toxic stimulation component in the prepared pinellia tuber slices through the steps of punching, fumigating, soaking in hypertonic solution, stuffiness preparation of penetrating fluid, high-pressure treatment and the like, increases the content of aspartic acid with cough relieving and phlegm eliminating effects, and mainly comprises the following steps: firstly, taking fresh pinellia tuber, peeling, cleaning and cutting into slices with the thickness of 5-6mm, and firstly, uniformly pricking small holes with needles on the surface of a pinellia tuber slice, wherein the number of the small holes is 4-5, and the diameter of the small holes is 1.5-2 mm; secondly, fumigating the pinellia ternata slices treated in the step one by 120-150 ℃ water vapor for 30-60s, then soaking the pinellia ternata slices in 40% glucose solution for 40-60min, taking out the pinellia ternata slices, carrying out infrared drying for 5-10min, and filtering the glucose solution for later use; thirdly, mixing 2-5 parts by weight of the glucose solution soaked in the summer sheet in the second step, 15-20 parts by weight of disodium ethylene diamine tetraacetate, 5-7 parts by weight of aspartic acid and 30-50 parts by weight of water, and stirring until the solution is transparent to prepare penetrating fluid; fourthly, placing the penetrating fluid in a sprayer, uniformly spraying the dried pinellia ternata slices until the pinellia ternata slices are completely moistened, then stacking the moistened pinellia ternata slices in a transparent porcelain jar, sealing and placing the transparent porcelain jar at a place where natural light is transmitted, standing for 24-36 hours, then placing the pinellia ternata slices with the penetrating fluid which is 0.1-0.5 time of the weight of the pinellia ternata slices in a pressure container, pressing for 20-30 minutes under the pressure of 0.16-0.18MPa, taking out the slices, and carrying out infrared drying again until the water content of the pinellia ternata slices is less than or equal to 8 percent.
The technical problem of application No. CN201710798222.6 is: complex processing operation, high breakage rate of pinellia ternata, dark color and high production cost, and is not suitable for large-scale production.
In order to solve the defects, the invention researches a processing and preparation method and a detection method of a pinellia ternate production place by taking effective components of total alkaloids and total organic acids as detection indexes through a large number of experiments, the method is classified according to the diameter of the pinellia ternate, and processing technologies of lime mixing and lime leaching are respectively researched.
Disclosure of Invention
The invention aims to provide a processing and preparation process of pinellia ternata producing area
The processing and preparation process of pinellia ternate producing areas, provided by the invention, comprises the steps of classifying pinellia ternate crude drugs, soaking the pinellia ternate crude drugs in lime mixture or lime water in an amount of 5-15% by weight until the outer skins of the pinellia ternate are slightly rotten, peeling the pinellia ternate crude drugs, and drying the pinellia ternate crude drugs at the temperature of 30-50 ℃ to obtain the pinellia ternate producing areas.
Preferably, the processing and preparation process of pinellia ternate producing areas, provided by the invention, is specifically that pinellia ternate crude drugs are taken to be subjected to size classification, then are soaked in lime mixture or lime water with the weight ratio of 5%, and are peeled and dried at the temperature of 35 ℃ to obtain the pinellia ternate producing areas.
The pinellia ternata crude drug is taken for size grading, and the difference of specific size grading diameters R is 0.5 cm.
The crude pinellia tuber medicine is taken for size grading, and the grading is carried out according to the diameter R <1.0cm, R <1.0cm < 1.5cm, R < 1.5cm < 2cm, and R >2.0 cm.
The lime water is soaked and fermented, and the dosage of the lime water is specifically as follows: r is less than 1.0cm, and the lime water is 0.5-1cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.5-1cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.5-1cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Preferably, the lime water is soaked and fermented, and the dosage of the lime water is specifically as follows: r is less than 1.0cm, and the lime water is 1cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 1cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 1cm higher than the surface of the medicinal materials; r is more than 2.0cm, and the lime water is flush with the medicine surface.
The invention also aims to provide a method for detecting the quality of the pinellia ternata.
The detection method is used for detecting the product prepared by the pinellia ternate producing area processing and preparing process, and specifically comprises the following steps: the content of total organic acid is determined by titration method, the content of total alkaloids is determined by ultraviolet-visible spectrophotometer method, and the water content is determined by drying method.
The specific method for determining the content of the total organic acid by adopting a titration method in the method for detecting the quality of the pinellia ternata comprises the following steps: precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder into a triangular conical flask, adding 10-50mL of 40-80% ethanol, weighing the weight, performing reflux extraction for 0.5-2.5h, cooling, complementing the weight, filtering, precisely weighing 4-6mL of pinellia ternate powder, adding 1 drop of 0.8-1.2% phenolphthalein solution, titrating with 0.995-0.105mg/mL of sodium hydroxide solution, recording the amount of NaOH, and calculating to obtain the finished product.
Preferably, the specific method for determining the content of the total organic acids by a titration method in the method for detecting the quality of the pinellia ternata comprises the following steps: the specific method for measuring the content of the total organic acid by adopting a titration method comprises the following steps: precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 50mL of 70% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
The specific method for measuring the content of the total alkaloids by adopting an ultraviolet-visible spectrophotometer in the method for detecting the quality of the pinellia ternata comprises the following steps: 0.5g of sample powder is precisely weighed and placed in a 50mL triangular flask, 0.5mL of concentrated ammonia water is added, 10mL of chloroform is added after wetting, and the mixture is cold-soaked for 3 hours. Performing ultrasonic treatment for 30min, filtering, washing the residue with 10mL of chloroform for 3 times, combining the filtrate and the washing solution, recovering the chloroform to dryness, adding 10mL of chloroform to dissolve the chloroform and transferring the chloroform to a 50mL separating funnel, precisely adding 10mL of buffer solution with pH6.0 and 1mL of bromothymol blue standard solution, fully shaking, standing for 30min, separating a chloroform layer, extracting a water layer twice by the same method with chloroform, combining 10mL of chloroform layers each time, recovering the chloroform to dryness, dissolving the residue with chloroform, placing in a 25mL measuring flask, diluting to a scale with chloroform, and shaking uniformly to obtain a sample solution. The test solution is measured on an ultraviolet-visible spectrophotometer under the condition of using chloroform as a blank and the wavelength of 413nm, and the absorbance is recorded.
The invention has the advantages of
(1) The invention optimizes the most preferable conditions of the pinellia ternate producing area processing technology through comprehensive evaluation: grading rhizoma Pinelliae at a distance of 0.5cm, mixing with 5% lime, peeling, and oven drying at 35 deg.C.
(2) The processing technology optimizes the production process of the pinellia ternate, adopts a processing method of directly stirring with lime or soaking in lime, has simple technology and convenient operation, changes the prior direct stacking traditional method, shortens the processing time, reduces the loss of effective components, improves the appearance and the internal quality of the product, ensures the stability and the reproducibility of variety technology, shows the reasonability and the feasibility of the processing technology of the researched producing area, provides a reference for formulating the quality standard of the decoction pieces of the pinellia ternate in the future, lays a foundation for further researching the producing area processing and the application of the pinellia ternate, and is suitable for large-scale industrial production.
(3) The research processing method determines the size grading parameters of the medicinal materials, ensures the uniformity, stability and effectiveness of processed products, and saves the processing cost of pinellia ternata.
(4) According to the research result, in the lime water soaking fermentation, the R of pinellia ternata is less than 1.0cm, the lime water is higher than the medicinal material surface, and the content of total organic acid is higher; r is more than or equal to 1.0cm and less than or equal to 1.5cm, the lime water is lower than the medicine surface, and the content of the total organic acid is higher; r is more than 1.5cm and less than or equal to 2cm, the lime water is higher than the medicinal material surface, and the content of the total organic acid is higher; r is more than 2.0cm, the lime water is flush with the surface of the medicinal material, and the content of the total organic acid is higher; the processing technology of the rhizoma pinelliae decoction pieces soaked in lime has no obvious rule on different lime dosages and total alkaloid contents.
(5) The research result shows that the content of the total organic acid in the pinellia ternata with the same diameter is reduced along with the increase of the lime consumption, so that the content of the total organic acid with the lime consumption of 5 percent is higher in the pinellia ternata with the same diameter; in pinellia ternata with the same diameter, the dosage of lime has little influence on the moisture content of the pinellia ternata.
(6) The method has the advantages of simple and easy process, easy peeling in the fermentation process, low breakage rate, white color and fresh color of the finished product, and high content of total alkaloids and total organic acids, and is stable, reasonable and feasible, and provides high value for guiding the production of pinellia ternata medicinal materials.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1: taking crude pinellia ternata, classifying, respectively taking 500kg of pinellia ternata with the diameter R of less than 1.0cm, R of less than or equal to 1.0cm and less than or equal to 1.5cm, R of less than or equal to 1.5cm and less than or equal to 2cm and R of more than 2.0cm, respectively stirring and fermenting with 25kg of lime, peeling, and drying at 35 ℃ to obtain the traditional Chinese medicine.
Example 2: after crude pinellia ternata is subjected to size classification, 500kg of pinellia ternata with the diameter R of less than 1.0cm, R of more than or equal to 1.0cm and less than or equal to 1.5cm, R of more than or equal to 1.5cm and less than or equal to 2cm and R of more than 2.0cm are respectively soaked and fermented by 25kg of lime and water until the pinellia ternata skin is slightly rotten, and the pinellia ternata is peeled and dried at the temperature of 35 ℃ to obtain the pinellia ternata fermented wine. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 1cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 1cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 1cm higher than the surface of the medicinal materials; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 3: grading crude drug of rhizoma Pinelliae, respectively weighing 500kg rhizoma Pinelliae with diameter of less than 1.0cm, diameter of 1.0cm or less than 1.5cm, diameter of 1.5cm or less than 2cm, and diameter of 2.0cm, respectively, stirring with 25kg lime, fermenting, peeling, and oven drying at 30 deg.C.
Example 4: the method comprises the steps of taking crude pinellia tuber, carrying out size classification, respectively taking 500kg of pinellia tuber with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm after the crude pinellia tuber is subjected to size classification, respectively soaking and fermenting the pinellia tuber with 25kg of lime and water until the outer skin of the pinellia tuber is slightly rotten, peeling the pinellia tuber, and drying. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 1cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 1cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 1cm higher than the surface of the medicinal materials; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 5: grading crude drug of rhizoma Pinelliae, respectively weighing 500kg rhizoma Pinelliae with diameter of less than 1.0cm, diameter of 1.0cm or less than 1.5cm, diameter of 1.5cm or less than 2cm, and diameter of 2.0cm, respectively, stirring with 25kg lime, fermenting, peeling, and oven drying at 50 deg.C.
Example 6: the preparation method comprises grading crude drug of rhizoma Pinelliae in size, respectively soaking 500kg rhizoma Pinelliae with diameter of less than 1.0cm, diameter of 1.0cm or less than 1.5cm, diameter of 1.5cm or less than 2cm, and diameter of 2.0cm in 25kg lime in water, fermenting until the outer skin of rhizoma Pinelliae is slightly rotten, peeling, and oven drying at 50 deg.C. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 1cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 1cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 1cm higher than the surface of the medicinal materials; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 7: taking crude pinellia ternata for size classification, respectively taking 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively stirring and fermenting with 75kg of lime, peeling, and drying at 35 ℃ to obtain the traditional Chinese medicine.
Example 8: the method comprises the steps of taking crude pinellia tuber to perform size classification, respectively taking 500kg of pinellia tuber with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively soaking and fermenting the pinellia tuber with 75kg of lime in water until the outer skin of the pinellia tuber is slightly rotten, peeling the pinellia tuber, and drying at the temperature of 35 ℃ to obtain the pinellia tuber. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 0.5cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.5cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.5cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 9: taking crude pinellia ternata for size classification, respectively taking 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively stirring and fermenting with 50kg of lime, peeling, and drying at 30 ℃ to obtain the traditional Chinese medicine.
Example 10: after crude pinellia ternata is subjected to size classification, 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm are respectively soaked and fermented in 50kg of lime and water until the outer skin of the pinellia ternata is slightly rotten, and the pinellia ternata is peeled and dried at the temperature of 30 ℃ to obtain the pinellia ternata fermented food. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 0.5cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.5cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.5cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 11: grading crude pinellia ternate, respectively taking 500kg of pinellia ternate with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively stirring and fermenting with 40kg of lime, peeling, and drying at 40 ℃ to obtain the traditional Chinese medicine.
Example 12: the preparation method comprises the steps of grading crude pinellia ternate in size, respectively taking 500kg of pinellia ternate with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively soaking and fermenting the pinellia ternate with 40kg of lime and water until the outer skin of the pinellia ternate is slightly rotten, peeling, and drying at the temperature of 40 ℃ to obtain the pinellia ternate. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 0.8cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.8cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.8cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 13: grading crude drug of rhizoma Pinelliae, respectively weighing 500kg rhizoma Pinelliae with diameter of less than 1.0cm, diameter of 1.0cm or less than 1.5cm, diameter of 1.5cm or less than 2cm, and diameter of 2.0cm, respectively, stirring with 25kg lime, fermenting, peeling, and oven drying at 45 deg.C.
Example 14: the preparation method comprises the steps of grading crude pinellia ternate in size, respectively taking 500kg of pinellia ternate with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than or equal to 2cm and the diameter of more than 2.0cm, respectively soaking and fermenting the pinellia ternate with 25kg of lime and water until the outer skin of the pinellia ternate is slightly rotten, peeling, and drying at 45. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 0.9cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.9cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.9cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 15: taking crude pinellia ternata for size classification, respectively taking 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively stirring and fermenting with 50kg of lime, peeling, and drying at 30 ℃ to obtain the traditional Chinese medicine.
Example 16: after crude pinellia ternata is subjected to size classification, 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm are respectively soaked and fermented in 50kg of lime and water until the outer skin of the pinellia ternata is slightly rotten, and the pinellia ternata is peeled and dried at the temperature of 30 ℃ to obtain the pinellia ternata fermented food. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 1cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 1cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 1cm higher than the surface of the medicinal materials; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 17: taking crude pinellia ternata for size classification, respectively taking 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively stirring and fermenting with 45kg of lime, peeling, and drying at 35 ℃ to obtain the traditional Chinese medicine.
Example 18: after crude pinellia ternata is subjected to size classification, 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm are respectively soaked and fermented in 45kg of lime and water until the outer skin of the pinellia ternata is slightly rotten, and the pinellia ternata is peeled and dried at the temperature of 35 ℃ to obtain the pinellia ternata fermented food. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 0.6cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.6cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.6cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 19: taking crude pinellia ternata for size classification, respectively taking 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively stirring and fermenting with 50kg of lime, peeling, and drying at 48 ℃ to obtain the traditional Chinese medicine.
Example 20: after crude pinellia ternata is subjected to size classification, 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm are respectively soaked and fermented in 50kg of lime and water until the outer skin of the pinellia ternata is slightly rotten, and the pinellia ternata is peeled and dried at 48 ℃ to obtain the pinellia ternata fermented food. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 0.7cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.7cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.7cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 21: taking crude pinellia ternata for size classification, respectively taking 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively stirring and fermenting with 75kg of lime, peeling, and drying at 32 ℃ to obtain the traditional Chinese medicine.
Example 22: the method comprises the steps of taking crude pinellia tuber to perform size classification, respectively taking 500kg of pinellia tuber with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively soaking and fermenting the pinellia tuber with 75kg of lime in water until the outer skin of the pinellia tuber is slightly rotten, peeling the pinellia tuber, and drying at the temperature of 32 ℃ to obtain the pinellia tuber. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 0.8cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.8cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.8cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 23: grading crude drug of rhizoma Pinelliae, respectively weighing 500kg rhizoma Pinelliae with diameter of less than 1.0cm, diameter of 1.0cm or less than 1.5cm, diameter of 1.5cm or less than 2cm, and diameter of 2.0cm, respectively, stirring with 30kg lime, fermenting, peeling, and oven drying at 43 deg.C.
Example 24: the preparation method comprises the steps of grading crude pinellia tuber according to size, respectively taking 500kg of pinellia tuber with diameter less than 1.0cm, diameter less than or equal to 1.5cm and diameter less than or equal to 1.0cm, diameter less than or equal to 2cm and diameter greater than 2.0cm, respectively soaking 30kg of lime in water, fermenting until the outer skin of the pinellia tuber is slightly rotten, peeling, and drying at 43 ℃ to obtain the final product. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 1cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 1cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 1cm higher than the surface of the medicinal materials; r is more than 2.0cm, and the lime water is flush with the medicine surface. .
Example 25: taking crude pinellia ternata for size classification, respectively taking 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively stirring and fermenting with 75kg of lime, peeling, and drying at 38 ℃ to obtain the traditional Chinese medicine.
Example 26: the method comprises the steps of taking crude pinellia tuber to perform size classification, respectively taking 500kg of pinellia tuber with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively soaking and fermenting the pinellia tuber with 75kg of lime in water until the outer skin of the pinellia tuber is slightly rotten, peeling the pinellia tuber, and drying at 38 ℃ to obtain the pinellia tuber. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 0.9cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.9cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.9cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Example 27: taking crude pinellia ternata for size classification, respectively taking 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively stirring and fermenting with 75kg of lime, peeling, and drying at 50 ℃ to obtain the traditional Chinese medicine.
Example 28: the method comprises the steps of taking crude pinellia tuber to perform size classification, respectively taking 500kg of pinellia tuber with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively soaking and fermenting the pinellia tuber with 75kg of lime in water until the outer skin of the pinellia tuber is slightly rotten, peeling the pinellia tuber, and drying at 50 ℃ to obtain the pinellia tuber. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 0.6cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.6cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.6cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface. .
Example 29: taking crude pinellia ternata for size classification, respectively taking 500kg of pinellia ternata with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively stirring and fermenting with 75kg of lime, peeling, and drying at 44 ℃ to obtain the traditional Chinese medicine.
Example 30: the method comprises the steps of taking crude pinellia tuber to perform size classification, respectively taking 500kg of pinellia tuber with the diameter of less than 1.0cm, the diameter of less than or equal to 1.0cm and less than or equal to 1.5cm, the diameter of less than or equal to 1.5cm and the diameter of more than 2.0cm, respectively soaking and fermenting the pinellia tuber with 75kg of lime in water until the outer skin of the pinellia tuber is slightly rotten, peeling the pinellia tuber, and drying at 44 ℃ to obtain the pinellia tuber. The lime water dosage is as follows: r is less than 1.0cm, and the lime water is 0.5cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.5cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.5cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
Examples 1-30 were each tested according to the quality test method for pinellia ternata of examples 31, 32, 33, 34, 35, 36, 37, 38, 39 and 40, respectively.
Example 31: pinellia ternata quality detection method
(1) Determination of total organic acid content by titration
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 50mL of 70% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
(2) Measuring total alkaloid content by ultraviolet-visible spectrophotometer
Preparing a reference substance: precisely weighing appropriate amount of ephedrine hydrochloride reference, dissolving with chloroform to obtain 0.0336mg/mL reference solution.
0.5g of sample powder is precisely weighed and placed in a 50mL triangular flask, 0.5mL of concentrated ammonia water is added, 10mL of chloroform is added after wetting, and the mixture is cold-soaked for 3 hours. Performing ultrasonic treatment for 30min, filtering, washing the residue with 10mL of chloroform for 3 times, combining the filtrate and the washing solution, recovering the chloroform to dryness, adding 10mL of chloroform to dissolve the chloroform and transferring the chloroform to a 50mL separating funnel, precisely adding 10mL of buffer solution with pH6.0 and 1mL of bromothymol blue standard solution, fully shaking, standing for 30min, separating a chloroform layer, extracting a water layer twice by the same method with chloroform, combining 10mL of chloroform layers each time, recovering the chloroform to dryness, dissolving the residue with chloroform, placing in a 25mL measuring flask, diluting to a scale with chloroform, and shaking uniformly to obtain a sample solution. Measuring the test solution on an ultraviolet-visible spectrophotometer with chloroform as a blank and a wavelength of 413nm, and recording the absorbance; (3) determination of moisture by drying
Drying the clean flat bottle at 105 deg.C for 5 hr, cooling in a drier for 30min, quickly and precisely weighing, drying at the above temperature for 1 hr, cooling, weighing, and weighing twice continuously with weighing difference of 0.3mg to obtain constant-weight flat bottle. Taking about 2g of a test article, paving the test article in a flat weighing bottle which is dried to constant weight, precisely weighing, opening a bottle cap, drying at 100-105 ℃ for 5 hours, covering the bottle cap, moving the bottle cap into a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference between two successive weighing is not more than 5mg, and calculating the water content in the test article according to the weight loss.
Example 32: pinellia ternata quality detection method
(1) Determination of total organic acid content by titration
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 50mL of 40% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with 0.995mg/mL of sodium hydroxide solution, recording the dosage of NaOH, and calculating to obtain the finished product. (2) Measuring total alkaloid content by ultraviolet-visible spectrophotometer
The same as in example 31.
(3) Determination of moisture by drying
The same as in example 31.
Example 33: pinellia ternata quality detection method
(1) Determination of total organic acid content by titration
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 40mL of 50% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
(2) Measuring total alkaloid content by ultraviolet-visible spectrophotometer
The same as in example 31.
(3) Determination of moisture by drying
The same as in example 31.
Example 34: pinellia ternata quality detection method
(1) Determination of total organic acid content by titration
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 30mL of 60% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
(2) Measuring total alkaloid content by ultraviolet-visible spectrophotometer
The same as in example 31.
(3) Determination of moisture by drying
The same as in example 31.
Example 35: pinellia ternata quality detection method
(1) Determination of total organic acid content by titration
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 20mL of 80% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
(2) Measuring total alkaloid content by ultraviolet-visible spectrophotometer
The same as in example 31.
(3) Determination of moisture by drying
The same as in example 31.
Example 36: pinellia ternata quality detection method
(1) Determination of total organic acid content by titration
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 50mL of 50% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
(2) Measuring total alkaloid content by ultraviolet-visible spectrophotometer
The same as in example 31.
(3) Determination of moisture by drying
The same as in example 31.
Example 37: pinellia ternata quality detection method
(1) Determination of total organic acid content by titration
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 10mL of 80% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
(2) Measuring total alkaloid content by ultraviolet-visible spectrophotometer
The same as in example 31.
(3) Determination of moisture by drying
The same as in example 31.
Example 38: pinellia ternata quality detection method
(1) Determination of total organic acid content by titration
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 70mL of 40% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
(2) Measuring total alkaloid content by ultraviolet-visible spectrophotometer
The same as in example 31.
(3) Determination of moisture by drying
The same as in example 31.
Example 39: pinellia ternata quality detection method
(1) Determination of total organic acid content by titration
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 70mL of 30% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
(2) Measuring total alkaloid content by ultraviolet-visible spectrophotometer
The same as in example 31.
(3) Determination of moisture by drying
The same as in example 31.
Example 40: pinellia ternata quality detection method
(1) Determination of total organic acid content by titration
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 70mL of 70% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
(2) Measuring total alkaloid content by ultraviolet-visible spectrophotometer
The same as in example 31.
(3) Determination of moisture by drying
The same as in example 31.
To further confirm the feasibility of the present invention, the inventors have verified through a number of experiments, and specific examples are as follows:
1 laboratory instruments and reagents
1.1 Experimental instruments
Electronic analytical balance (Mettler-Tolliduo instruments Co., Ltd.: GB/T23111), electric heat forced air drying box (Testet instruments Co., Ltd., Tianjin city: 101-2AB), digital display constant temperature water bath (Changzhou Australian instruments Co., Ltd.: HH-2), ultrasonic cleaning machine (Shanghai Yi Jing ultrasonic instruments Co., Ltd.: 164011221), ultraviolet-visible spectrophotometer (Beijing Pujingyo instruments Co., Ltd.: TU-1810)
1.2 reference substance
Ephedrine hydrochloride (purchased from China institute for testing biological products of drugs, batch number: 0714-
1.3 reagents
Sodium hydroxide (batch number of Chongqing Jiang Chuan chemical Co., Ltd.: 2017, 1 month and 3 days), absolute ethyl alcohol (batch number of analytical pure Tianjin Yongcheng fine chemical Co., Ltd.: 2017, 7 month and 29 days), phenolphthalein (batch number of Tianjin Yongcheng fine chemical Co., Ltd.), bromothymol blue (batch number of Dengzhou chemical reagent Co., Ltd.: 2010, 10 months and 29 days), sodium acetate (batch number of Xilonga chemical reagent Co., Ltd.: 1310111), trichloromethane (batch number of Shanghai Shenbo chemical Co., Ltd.: 1709101), ammonia water (batch number of Chongqing Jiang Chuan chemical Co., Ltd.: 20140310), glacial acetic acid (batch number of Tianjin Kou Miou North chemical reagent Co., Ltd.: 20170510) and the like are all analytically pure, and the experimental water is distilled water.
2 sources of samples
The medicinal materials are purchased in the four villages of river town in Chachi county of Hechapter city of Bijie city of Guizhou province in 2017 months and 9 months respectively, and are identified as the root tuber of Pinellia ternate Pinellia terrata (thunnb.) Breit.
3 sample preparation
3.1 different sizes of diameter pinellia Tuber
Taking the same batch of crude pinellia tuber medicine, and dividing the crude pinellia tuber medicine into the following components according to the diameter (R): r is less than 1.0cm, R is less than or equal to 1.5cm and is more than or equal to 1.0cm, R is less than or equal to 2cm and R is more than or equal to 2.0cm and is less than or equal to 1.5cm and is less than or equal to 2cm, R is more than or equal to 2.0cm) by respectively peeling by the methods of 3.2 and 3.3, and drying to obtain.
3.2 lime usage in different proportions
Mixing rhizoma Pinelliae with the same diameter with 5%, 10% and 15% (based on rhizoma Pinelliae weight) calx respectively, fermenting, peeling, and oven drying.
3.3 different limewater dosages
Soaking rhizoma Pinelliae with the same diameter in lime water 0.5-1cm below the medicinal material surface, equal to the medicinal material surface, and 0.5-1cm above the medicinal material surface, fermenting, peeling, and oven drying.
3.4 different drying temperatures
Taking crude pinellia ternata with the same diameter, mixing with lime, soaking in lime water, peeling, and oven drying at 30 deg.C, 35 deg.C, 40 deg.C, 45 deg.C, and 50 deg.C.
4 methods and results
4.1 Total organic acid content measurement
4.1.1 examination of extraction conditions
4.1.1.1 investigation of solvent for extraction: precisely weighing about 1.0g of pinellia tuber powder, placing the pinellia tuber powder into a triangular conical flask, respectively adding 30mL of distilled water and 30mL of 80% ethanol solution, weighing the weight, carrying out reflux extraction for 30min, complementing the weight, filtering, precisely weighing 5mL of subsequent filtrate, adding 1 drop of 1% phenolphthalein solution, titrating with 0.10175mg/mL of sodium hydroxide solution, and recording the dosage of the sodium hydroxide solution, wherein each sample is used for three times in parallel. The results are shown in Table 1.
TABLE 1 examination and examination of the extraction solvent
The results show that the total organic acid content in the alcohol extraction is higher.
4.1.1.2 investigation of solvent dosage: weighing about 1.0g of pinellia ternate powder accurately, placing the pinellia ternate powder into a triangular conical flask, adding 10 times, 20 times, 30 times, 40 times and 50 times of 80% ethanol solution respectively, weighing, refluxing for 30min, taking out, cooling, complementing the weight, filtering, accurately weighing a subsequent filtrate 1/5, fixing the volume to a scale mark in a 10mL volumetric flask, adding 1 drop of 1% phenolphthalein solution, titrating with 0.10175mg/mL sodium hydroxide solution, recording the dosage of the sodium hydroxide solution, and paralleling each sample for three times. The results are shown in Table 2.
Table 2 investigation of solvent dosage experimental results
The result shows that the content of the total organic acid is increased along with the increase of the dosage of the solvent, but the content of the total organic acid is not greatly different from that of the solvent 40 times when the solvent is 50 times, so that the dosage of the solvent is only 50 times for researching the cost-saving factor.
4.1.1.3 investigation of solvent concentration for extraction: weighing about 1.0g of pinellia tuber powder accurately, placing the pinellia tuber powder into a triangular conical flask, adding 30mL of 40%, 50%, 60%, 70% and 80% ethanol solution respectively, weighing, refluxing for 30min, taking out, cooling, complementing the weight, filtering, accurately weighing 5mL of subsequent filtrate, adding 1 drop of 1% phenolphthalein solution, titrating with sodium hydroxide solution with the concentration of 0.10175mg/mL, and recording the dosage of the sodium hydroxide solution, wherein each sample is carried out in parallel for three times. The results are shown in Table 3.
TABLE 3 investigation of the concentration of extraction solvent
The results show that 50%, 60% and 70% of total organic acid extracted by the method is higher in content.
4.1.1.4 investigation of extraction time: weighing about 1.0g of pinellia tuber powder accurately, placing the pinellia tuber powder into a triangular conical flask, adding 30mL of 80% ethanol solution, weighing, refluxing for 0.5h, 1.0h, 1.5h, 2.0h and 2.5h respectively, taking out, cooling, complementing the weight, filtering, accurately weighing 5mL of subsequent filtrate, adding 1 drop of 1% phenolphthalein solution, titrating with 0.10175mg/mL sodium hydroxide solution, recording the dosage of the sodium hydroxide solution, and paralleling each sample for three times. The results are shown in Table 4.
TABLE 4 extraction of time study test results
The results show that the total organic acid content is higher when the extraction time is 1, 1.5 and 2 hours.
4.1.2 orthogonal assay: 3 factors of the amount (A) of the extraction solvent, the concentration (B) of the extraction solvent and the extraction time (C) were selected as single factor subjects, and the factor levels are shown in Table 5 by an L9(3)4 orthogonal test.
TABLE 5 levels of factors
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder into a triangular conical flask, extracting according to the conditions of the following orthogonal test table, taking out the pinellia ternate powder after extraction, cooling, complementing the weight, filtering, precisely weighing 5mL of continuous filtrate, adding 1 drop of 1% phenolphthalein solution, titrating with sodium hydroxide solution with the concentration of 0.10175mg/mL, and recording the dosage of the sodium hydroxide solution, wherein each sample is paralleled for three times. The orthogonal experiment table and the orthogonal experiment result are shown in table 6.
TABLE 6 orthogonal experiments and results table
The optimal process condition obtained by range analysis is A3B3C3。
Table 7 for analysis of variance.
TABLE 7 ANOVA TABLE
The results show that pole A>B>C, the amount of the extraction solvent, the concentration of the extraction solvent and the extraction time are the most greatly influenced by the content of the total organic acid in the summerherb, and the optimal extraction condition is A by combining visual analysis and variance analysis3B3C3Namely, 50 times of solvent is added, the concentration of the solvent is 70 percent, and the extraction time is 2.0 h. While P is known from ANOVA>0.05 no significant difference.
4.2 verification of extraction Process
Precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder into a triangular conical flask, adding 70% ethanol, weighing 50mL of the weight, performing reflux extraction for 2.0h, cooling, complementing the weight, filtering, precisely weighing 5mL of each sample solution, adding 1 drop of 1% phenolphthalein solution, titrating with 0.10175mg/mL sodium hydroxide solution, recording the amount of NaOH, and performing three times in parallel. The results are shown in Table 8.
TABLE 8 table of results of confirmatory tests
Through the positive cross validation test, the highest value of the results in the orthogonal test table can be achieved, and the optimal processing process condition selected by the orthogonal test is stable, so that the method for processing the pinellia ternata has feasibility.
4.2.1 sample determination
4.2.1.1 measurement of Total organic acid content
Precisely weighing 0.1g of each sample pinellia ternate powder, placing the pinellia ternate powder into a triangular conical flask, adding 70% ethanol, weighing 50mL of the weight, refluxing and extracting for 2.0h, cooling, complementing the weight, filtering, precisely weighing 5mL of each sample solution, adding 1 drop of 1% phenolphthalein solution, titrating with sodium hydroxide solution with the concentration of 0.10175mg/mL, and recording the dosage of NaOH.
4.2.1.2 moisture determination
Drying the clean flat bottle at 105 deg.C for 5 hr, cooling in a drier for 30min, quickly and precisely weighing, drying at the above temperature for 1 hr, cooling, weighing, and weighing twice continuously with weighing difference of 0.3mg to obtain constant-weight flat bottle. Taking about 2g of a test article, paving the test article in a flat weighing bottle which is dried to constant weight, precisely weighing, opening a bottle cap, drying at 100-105 ℃ for 5 hours, covering the bottle cap, moving the bottle cap into a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference between two successive weighing is not more than 5mg, and calculating the water content in the test article according to the weight loss.
4.2.1.3 Total alkaloid content determination
0.5g of sample powder is precisely weighed and placed in a 50mL triangular flask, 0.5mL of concentrated ammonia water is added, 10mL of chloroform is added after wetting, and the mixture is cold-soaked for 3 hours. Performing ultrasonic treatment for 30min, filtering, washing the residue with 10mL of chloroform for 3 times, combining the filtrate and the washing solution, recovering the chloroform to dryness, adding 10mL of chloroform to dissolve the chloroform and transferring the chloroform to a 50mL separating funnel, precisely adding 10mL of buffer solution with pH6.0 and 1mL of bromothymol blue standard solution, fully shaking, standing for 30min, separating a chloroform layer, extracting a water layer twice by the same method with chloroform, combining 10mL of chloroform layers each time, recovering the chloroform to dryness, dissolving the residue with chloroform, placing in a 25mL measuring flask, diluting to a scale with chloroform, and shaking uniformly to obtain a sample solution. The test solution is measured on an ultraviolet-visible spectrophotometer under the condition of using chloroform as a blank and the wavelength of 413nm, and the absorbance is recorded.
Preparing a reference substance: precisely weighing 11.08mg of ephedrine hydrochloride control dried at 105 deg.C to constant weight, placing in 50ml measuring flask, adding distilled water to dissolve, diluting to scale, and shaking to obtain ephedrine hydrochloride control solution (containing 0.2216mg of ephedrine hydrochloride per 1 ml).
Drawing a standard curve: sequentially taking 1mL, 2.5mL, 4mL, 5.5mL, 7mL, 8.5mL and 10mL of ephedrine hydrochloride reference substance solution, respectively adding distilled water to 10mL, placing in a 50mL separating funnel, precisely adding 10mL of buffer solution and 1mL of bromothymol blue standard solution, adding 10mL of chloroform, fully shaking, standing for 30min, separating a chloroform layer, and extracting the water layer twice by the same method with chloroform, 10mL each time. And combining the chloroform layers, recovering to dryness, dissolving the residue with chloroform, placing into a 25mL measuring flask, diluting to the scale with chloroform, and shaking up to obtain the solution to be detected. The absorbance was measured at 413nm with chloroform as a blank. The absorbance was plotted as the ordinate and the concentration was plotted as the abscissa to obtain a standard curve, and the results are shown in Table 9.
TABLE 9 Standard Curve plotting the results (n ═ 7)
As can be seen from Table 9, the linear relationship between the total alkali of pinellia tuber and 0.0082 mg/ml-0.082 mg/ml is good, and the working curve equation is obtained: a is 3.7776C +0.4581, R2 is 0.9993 (absorbance at position a, C is concentration).
Preferred results of 5-generation process conditions
5.1 index content Total organic acid and moisture content are preferred
5.1.1. determination of total organic acid content of different lime dosages in the processing technology of lime-mixed pinellia tuber decoction pieces:
pinellia ternata crude drugs with different diameters are selected and classified according to the diameter R, and pinellia ternata decoction pieces are respectively processed according to a lime mixing processing technology under the item of sample processing in 3 groups per grade. Precisely weighing 0.1g of each sample pinellia ternate powder, placing the pinellia ternate powder into a triangular conical flask, adding 70% ethanol, weighing 50mL of the weight, refluxing and extracting for 2.0h, cooling, complementing the weight, filtering, precisely weighing 5mL of each sample solution, adding 1 drop of 1% phenolphthalein solution, titrating with 0.10175mg/mL sodium hydroxide solution, and recording the dosage of NaOH to measure the total organic acid.
Drying the clean flat bottle at 105 deg.C for 5 hr, cooling in a drier for 30min, quickly and precisely weighing, drying at the above temperature for 1 hr, cooling, weighing, and weighing twice continuously with weighing difference of 0.3mg to obtain constant-weight flat bottle. Taking about 2g of a test article, paving the test article in a flat weighing bottle which is dried to constant weight, precisely weighing, opening a bottle cap, drying for 5 hours at the temperature of 100-105 ℃, covering the bottle cap, moving the bottle cap into a dryer, cooling for 30 minutes, precisely weighing, drying for 1 hour at the temperature, cooling, weighing until the difference between two successive weighing is not more than 5mg, and calculating the water content in the test article according to the weight loss to carry out water content determination. The results and analysis are shown in Table 10.
TABLE 10 determination of total organic acid content for different lime dosages in lime mixing process
The results show that: the total organic acid content is reduced along with the increase of the lime consumption in the pinellia ternata with the same diameter, so that the total organic acid content is higher when the lime consumption is 5 percent in the pinellia ternata with the same diameter; ② in the pinellia tuber with the same diameter, the dosage of lime has little influence on the moisture content of the pinellia tuber.
Therefore, in the lime mixing processing technology, the content of the total organic acid is higher when the lime is used in an amount of 5%.
5.1.2 determination of total organic acid content by using different lime water in the processing technology of the lime soaked pinellia tuber decoction pieces:
selecting crude pinellia ternata medicines with different diameters, grading according to the diameter R, and processing into crude pinellia ternata medicines by using lime water 0.5-1cm higher than the medicine surface, leveling the medicine surface, and 0.5-1cm higher than the medicine surface according to lime soaking processing technology under the item of 'sample preparation' for each 3 groups. Precisely weighing 0.1g of each sample pinellia ternate powder, placing the pinellia ternate powder into a triangular conical flask, adding 70% ethanol, weighing 50mL of the weight, refluxing and extracting for 2.0h, cooling, complementing the weight, filtering, precisely weighing 5mL of each sample solution, adding 1 drop of 1% phenolphthalein solution, titrating with 0.10175mg/mL sodium hydroxide solution, and recording the dosage of NaOH to measure the total organic acid.
Drying the clean flat bottle at 105 deg.C for 5 hr, cooling in a drier for 30min, quickly and precisely weighing, drying at the above temperature for 1 hr, cooling, weighing, and weighing twice continuously with weighing difference of 0.3mg to obtain constant-weight flat bottle. Taking about 2g of a test article, paving the test article in a flat weighing bottle which is dried to constant weight, precisely weighing, opening a bottle cap, drying for 5 hours at the temperature of 100-105 ℃, covering the bottle cap, moving the bottle cap into a dryer, cooling for 30 minutes, precisely weighing, drying for 1 hour at the temperature, cooling, weighing until the difference between two successive weighing is not more than 5mg, and calculating the water content in the test article according to the weight loss to carry out water content determination. The results and analysis are shown in Table 11.
TABLE 11 determination of the Total organic acid content for different lime wash dosages in the lime leaching Process
The result shows that R of the pinellia ternata is less than 1.0cm, the lime water is higher than the medicinal material surface, and the content of the total organic acid is higher; r is more than or equal to 1.0cm and less than or equal to 1.5cm, the lime water is lower than the medicine surface, and the content of the total organic acid is higher; r is more than 1.5cm and less than or equal to 2cm, the lime water is higher than the medicinal material surface, and the content of the total organic acid is higher; r is more than 2.0cm, the lime water is flush with the surface of the medicinal material, and the content of the total organic acid is higher.
5.1.3 Total organic acid content determination at different drying temperatures:
the method comprises the steps of selecting two pinellia ternata crude drugs with different diameters, respectively dividing the two pinellia ternata crude drugs into 5 groups, and processing the pinellia ternata crude drugs by a direct peeling processing technology under the item of sample preparation.
And (3) total organic acid determination: precisely weighing 0.1g of each sample pinellia ternate powder, placing the pinellia ternate powder into a triangular conical flask, adding 70% ethanol, weighing 50mL of the weight, refluxing and extracting for 2.0h, cooling, complementing the weight, filtering, precisely weighing 5mL of each sample solution, adding 1 drop of 1% phenolphthalein solution, titrating with 0.10175mg/mL sodium hydroxide solution, and recording the dosage of NaOH to measure the total organic acid.
And (3) moisture determination: drying the clean flat bottle at 105 deg.C for 5 hr, cooling in a drier for 30min, quickly and precisely weighing, drying at the above temperature for 1 hr, cooling, weighing, and weighing twice continuously with weighing difference of 0.3mg to obtain constant-weight flat bottle. Taking about 2g of a test article, paving the test article in a flat weighing bottle which is dried to constant weight, precisely weighing, opening a bottle cap, drying at 100-105 ℃ for 5 hours, covering the bottle cap, moving the bottle cap into a dryer, cooling for 30 minutes, precisely weighing, drying at the temperature for 1 hour, cooling, weighing until the difference between two successive weighing is not more than 5mg, and calculating the water content in the test article according to the weight loss.
The total organic acid and water content are measured by the measuring method. The results and analysis are shown in Table 12.
TABLE 12 Total organic acid content determination at different stoving temperatures
The result shows that in the processing technology of the pinellia tuber producing area, the pinellia tuber decoction pieces with the drying temperature of 35 ℃ in the pinellia tuber with the same diameter have higher content of the total organic acid.
5.2 content of the total alkaloid
5.2.1 determination of content of total alkaloids by using different lime in processing technique of rhizoma Pinelliae decoction pieces mixed with lime
Selecting crude pinellia tuber drugs with different diameters, classifying according to the diameter R, classifying 3 groups per group, precisely weighing 0.5g of sample powder of pinellia tuber decoction pieces processed by lime mixing processing technology under the item of sample preparation, placing in a 50mL triangular flask, adding 0.5mL of concentrated ammonia water, moistening, adding 10mL of chloroform, and cold soaking for 3 h. Performing ultrasonic treatment for 30min, filtering, washing the residue with 10mL of chloroform for 3 times, combining the filtrate and the washing solution, recovering the chloroform to dryness, adding 10mL of chloroform to dissolve the chloroform and transferring the chloroform to a 50mL separating funnel, precisely adding 10mL of buffer solution with pH6.0 and 1mL of bromothymol blue standard solution, fully shaking, standing for 30min, separating a chloroform layer, extracting an aqueous layer twice by the same method with chloroform, 10mL each time, combining the chloroform layers, recovering the chloroform to dryness, dissolving the residue with chloroform, placing the solution in a 25mL measuring flask, diluting the solution to a scale by using chloroform, and shaking uniformly to obtain a sample solution. Measuring the test solution with chloroform as blank and wavelength of 413nm in ultraviolet-visible spectrophotometer, and recording absorbance to determine total alkaloid content. The results and analysis are shown in Table 13.
TABLE 13 determination of total alkaloid content in lime mixing process at different lime dosages
The result shows that in the lime mixing processing technology, when the dosage of pinellia tuber lime with the same diameter is mostly 5%, the total alkaloid content is the highest.
5.2.2 measurement of Total alkaloid content in different lime water dosage in processing technique of rhizoma Pinelliae decoction pieces soaked with lime
Selecting pinellia ternate crude drugs with different diameters for classification according to the diameter R, classifying 3 groups of pinellia ternate crude drugs, respectively processing pinellia ternate crude drugs by lime water which is 0.5cm higher than the surface of the crude drugs, is flush with the surface of the crude drugs, is 0.5cm higher than the surface of the crude drugs according to the lime soaking processing technology under the item of sample preparation, and adding 0.5g of pinellia ternate crude drug sample powder processed by the lime soaking processing technology under the item of sample preparation, precisely weighing, placing the pinellia ternate crude drug sample powder into a 50mL triangular flask, adding 0.5mL of concentrated ammonia water, moistening, adding 10mL of chloroform, and cold soaking for 3 hours. Performing ultrasonic treatment for 30min, filtering, washing the residue with 10mL of chloroform for 3 times, combining the filtrate and the washing solution, recovering the chloroform to dryness, adding 10mL of chloroform to dissolve the chloroform and transferring the chloroform to a 50mL separating funnel, precisely adding 10mL of buffer solution with pH6.0 and 1mL of bromothymol blue standard solution, fully shaking, standing for 30min, separating a chloroform layer, extracting an aqueous layer twice by the same method with chloroform, 10mL each time, combining the chloroform layers, recovering the chloroform to dryness, dissolving the residue with chloroform, placing the solution in a 25mL measuring flask, diluting the solution to a scale by using chloroform, and shaking uniformly to obtain a sample solution. Measuring the test solution with chloroform as blank and wavelength of 413nm in ultraviolet-visible spectrophotometer, and recording absorbance to determine total alkaloid content. The results and analysis are shown in Table 14.
TABLE 14 determination of total alkaloid content in lime leaching process at different lime dosages
The results show that the dosage of lime and the content of total alkaloids in the processing technology of the pinellia decoction pieces soaked in lime have no obvious rule.
5.2.3 measurement of Total alkaloid content at different oven-drying temperatures:
selecting two crude pinellia tuber medicines with different diameters, dividing into 5 groups, precisely weighing rhizoma Pinelliae decoction pieces processed by direct peeling processing under the item of sample preparation according to the sample powder of 0.5g, placing in a 50mL triangular flask, adding concentrated ammonia water of 0.5mL, moistening, adding chloroform of 10mL, and cold soaking for 3 h. Performing ultrasonic treatment for 30min, filtering, washing the residue with 10mL of chloroform for 3 times, combining the filtrate and the washing solution, recovering the chloroform to dry, adding 10mL of chloroform to dissolve, transferring to a 50mL separating funnel, precisely adding 10mL of buffer solution with pH of 6.0 and 1mL of bromothymol blue standard solution, fully shaking, standing for 30min, separating a chloroform layer, and extracting the water layer with chloroform twice, 10mL each time. Combining chloroform layers, recovering to dryness, dissolving the residue with chloroform, placing in a 25mL measuring flask, diluting to scale with chloroform, and shaking to obtain the test solution. Measuring the test solution on an ultraviolet-visible spectrophotometer with chloroform as blank and wavelength of 413nm, and recording absorbance to determine total alkaloid content. The results and analysis are shown in Table 15.
TABLE 15 measurement of Total alkaloid content at different oven-drying temperatures
The result shows that in the processing technology of the pinellia ternata producing area, different batches of pinellia ternata show that the pinellia ternata total alkaloid content of the pinellia ternata with the same diameter is higher at the drying temperature of 50 ℃.
5.3 general scoring optimization
According to the importance of the measured components, the total organic acid accounts for 0.3, the total alkaloid accounts for 0.7, and a comprehensive evaluation method is adopted, wherein the comprehensive evaluation value is 0.3 total organic acid + 0.7 total alkaloid, and the experimental results under the items that the index content is total organic acid optimization and the index content is total alkaloid optimization are comprehensively evaluated, so that the process conditions of the pinellia ternate producing area are optimized.
Investigating different lime consumption in the lime mixing process under a comprehensive grading method: the results are shown in Table 16.
TABLE 16 investigation of different lime dosages in lime blending Process under the comprehensive Scoring method
As can be seen from the above table, in the processing technology of the decoction pieces of pinellia ternata mixed with lime, the quality of pinellia ternata with the lime amount of 5% is better.
And (3) investigating different lime water dosage in the processing technology of the rhizoma pinelliae decoction pieces soaked in lime by a comprehensive scoring method: the results are shown in Table 17.
TABLE 17 investigation of different lime water usage in lime leaching process under comprehensive scoring method
The results show that the law of different lime water dosage and the comprehensive grade value of pinellia ternate in the processing technology of the decoction pieces of pinellia ternate soaked in lime is as follows:
1. aiming at different lime water usage amounts: in the specification that R is less than 1.0cm, the amount of the lime water is higher than the highest comprehensive score of the medicinal material surface; in the specification that R is more than or equal to 1.0 and less than or equal to 1.5, the consumption of the lime water is lower than the comprehensive score of the medicine surface and is the highest; in the specification that R is more than 1.5 and less than or equal to 2cm, the amount of the lime water is higher than the highest comprehensive score of the medicinal material surface; in the specification that R is larger than 2.0cm, the comprehensive score of the dosage of the lime water is the highest on the medicine surface.
2. In the same amount of lime water: the comprehensive score is lower than the medicine surface, the medicine specification is 1.5< R < 2cm, and the comprehensive score is highest; the medicine surface is leveled, and the comprehensive score is highest when the medicine specification R is more than 2.0 cm; the medicine is higher than the medicine powder, the medicine specification is 1.5< R < 2cm, and the comprehensive score is the highest.
Investigating different drying temperatures under a comprehensive grading method: the results are shown in Table 18.
TABLE 18 investigation of different drying temperatures under the comprehensive Scoring method
1. For the same temperature: the specification comprehensive score of R >2.0cm is highest at 30 ℃; the specification comprehensive score of R >2.0cm is highest at 35 ℃; at 40 ℃, comprehensively evaluating the specification of R >2.0cm and the specification of R < 1.5< 2 cm; the specification comprehensive score of R >2.0cm is highest at 45 ℃; the highest composite score for the specification with R >2.0cm is found at 50 ℃. Thus, the larger the specification, the higher the composite score at the same temperature. Therefore, it is recommended to perform the classification drying in the drying process to be favorable for high quality and high price.
2. In the same specification: in the specification that R is more than 2.0cm, the temperature is 35 ℃ and the comprehensive score is the highest; in the specification that R is more than 1.5 and less than or equal to 2cm, the comprehensive score is the highest when the temperature is 35 ℃. The result shows that the optimal drying temperature of the pinellia ternata is 35 ℃ in the same specification.
5.4 conclusion of the experiment
(1) In the production place processing process, the influence of the sizes of the pinellia ternate on the processing process is considered, so in the research process, the pinellia ternate with the diameter is graded according to the difference of 0.5cm, and the lime amount, the lime water amount and the drying temperature are considered on the basis of different grades.
(2) Analysis by experimental data: according to the condition that the effective components are evaluation indexes, the processing technology of the pinellia ternate producing area comprises the following steps: grading crude drug of rhizoma Pinelliae, mixing with 5% lime or soaking in lime, fermenting, peeling, and oven drying at 35 deg.C.
(3) The specific method for the content of the total organic acid of the pinellia ternata comprises the following steps: precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 50mL of 70% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
(4) The specific method for the content of the pinellia ternate total alkaloids comprises the following steps: 0.5g of sample powder is precisely weighed and placed in a 50mL triangular flask, 0.5mL of concentrated ammonia water is added, 10mL of chloroform is added after wetting, and the mixture is cold-soaked for 3 hours. Performing ultrasonic treatment for 30min, filtering, washing the residue with 10mL of chloroform for 3 times, combining the filtrate and the washing solution, recovering the chloroform to dryness, adding 10mL of chloroform to dissolve the chloroform and transferring the chloroform to a 50mL separating funnel, precisely adding 10mL of buffer solution with pH6.0 and 1mL of bromothymol blue standard solution, fully shaking, standing for 30min, separating a chloroform layer, extracting a water layer twice by the same method with chloroform, combining 10mL of chloroform layers each time, recovering the chloroform to dryness, dissolving the residue with chloroform, placing in a 25mL measuring flask, diluting to a scale with chloroform, and shaking uniformly to obtain a sample solution. The test solution is measured on an ultraviolet-visible spectrophotometer under the condition of using chloroform as a blank and the wavelength of 413nm, and the absorbance is recorded.
While the invention has been described in detail in the foregoing by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that certain changes and modifications may be made therein based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A processing and preparation process of pinellia ternate producing areas is characterized in that pinellia ternate crude drugs are taken to be subjected to size classification, then are soaked in lime or lime water with the weight ratio of 5-15% until the outer skins of the pinellia ternate are slightly rotten, are peeled, and are dried at the temperature of 30-50 ℃ to obtain the pinellia ternate producing areas.
2. The processing and preparation process of pinellia ternate producing area according to claim 1, wherein the crude pinellia ternate is prepared by the steps of size classification, soaking in 5% by weight of lime mixture or lime water until the outer skin of pinellia ternate is slightly rotten, peeling, and drying at 35 ℃.
3. The processing and preparation process of pinellia ternata production area according to any one of claims 1-2, wherein the crude pinellia ternata is taken for size classification, and the specific size classification diameter R difference is 0.5 cm.
4. A ban Xia Sheng Di preparation process according to any one of claims 1-2, characterized in that the ban Xia crude drug is classified according to its size, specifically according to the diameter R <1.0cm, R <1.0cm < R < 1.5cm, R < 1.5cm < R < 2cm, R >2.0 cm.
5. A pinellia ternata L production place processing and preparation process according to any one of claims 1 to 2, wherein the lime water is soaked and fermented, and the dosage of the lime water is specifically as follows: r is less than 1.0cm, and the lime water is 0.5-1cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 0.5-1cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 0.5-1cm higher than the medicinal material surface; r is more than 2.0cm, and the lime water is flush with the medicine surface.
6. A pinellia ternata L production place processing and preparation process according to any one of claims 1 to 2, wherein the lime water is soaked and fermented, and the dosage of the lime water is specifically as follows: r is less than 1.0cm, and the lime water is 1cm higher than the medicinal material surface; r is more than or equal to 1.0cm and less than or equal to 1.5cm, and the lime water is 1cm lower than the medicine surface; r is more than 1.5cm and less than or equal to 2cm, and the lime water is 1cm higher than the surface of the medicinal materials; r is more than 2.0cm, and the lime water is flush with the medicine surface.
7. A detection method for pinellia ternate quality is characterized by being used for detecting a product prepared by the pinellia ternate producing area processing and preparing process according to any one of claims 1 to 3, and specifically comprising the following steps of: the content of total organic acid is determined by titration method, the content of total alkaloids is determined by ultraviolet-visible spectrophotometer method, and the water content is determined by drying method.
8. The detection method according to claim 7, wherein the specific method for determining the content of the total organic acid by the titration method comprises the following steps: precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder into a triangular conical flask, adding 10-50mL of 40-80% ethanol, weighing the weight, performing reflux extraction for 0.5-2.5h, cooling, complementing the weight, filtering, precisely weighing 4-6mL of pinellia ternate powder, adding 1 drop of 0.8-1.2% phenolphthalein solution, titrating with 0.995-0.105mg/mL of sodium hydroxide solution, recording the amount of NaOH, and calculating to obtain the finished product.
9. The detection method according to claim 8, wherein the specific method for determining the content of the total organic acid by the titration method comprises the following steps: precisely weighing 0.1g of pinellia ternate powder, placing the pinellia ternate powder in a triangular conical flask, adding 50mL of 70% ethanol, weighing the weight, performing reflux extraction for 2h, cooling, complementing the weight, filtering, precisely weighing 5mL of the pinellia ternate powder, adding 1 drop of 1% phenolphthalein solution, titrating the solution with sodium hydroxide solution with the concentration of 0.10175mg/mL, recording the dosage of NaOH, and calculating to obtain the finished product.
10. The detection method according to claim 7, wherein the specific method for measuring the content of the total alkaloids by using an ultraviolet-visible spectrophotometer method comprises the following steps: 0.5g of sample powder is precisely weighed and placed in a 50mL triangular flask, 0.5mL of concentrated ammonia water is added, 10mL of chloroform is added after wetting, and the mixture is cold-soaked for 3 hours. Performing ultrasonic treatment for 30min, filtering, washing the residue with 10mL of chloroform for 3 times, combining the filtrate and the washing solution, recovering the chloroform to dryness, adding 10mL of chloroform to dissolve the chloroform and transferring the chloroform to a 50mL separating funnel, precisely adding 10mL of buffer solution with pH6.0 and 1mL of bromothymol blue standard solution, fully shaking, standing for 30min, separating a chloroform layer, extracting a water layer twice by the same method with chloroform, combining 10mL of chloroform layers each time, recovering the chloroform to dryness, dissolving the residue with chloroform, placing in a 25mL measuring flask, diluting to a scale with chloroform, and shaking uniformly to obtain a sample solution. The test solution is measured on an ultraviolet-visible spectrophotometer under the condition of using chloroform as a blank and the wavelength of 413nm, and the absorbance is recorded.
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