CN106248620A - A kind of numbness preparation is dried the method for quick of intermediate multi objective - Google Patents
A kind of numbness preparation is dried the method for quick of intermediate multi objective Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 77
- 231100000862 numbness Toxicity 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- -1 lactone glucoside Chemical class 0.000 claims abstract description 46
- 229930182470 glycoside Natural products 0.000 claims abstract description 26
- 229930183477 epimedin Natural products 0.000 claims abstract description 24
- 229930182478 glucoside Natural products 0.000 claims abstract description 23
- TZJALUIVHRYQQB-XFDQAQKOSA-N Icariin Natural products O(C)c1ccc(C2=C(O[C@H]3[C@@H](O)[C@H](O)[C@@H](O)[C@H](C)O3)C(=O)c3c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O4)c(C/C=C(\C)/C)c3O2)cc1 TZJALUIVHRYQQB-XFDQAQKOSA-N 0.000 claims abstract description 22
- TZJALUIVHRYQQB-XLRXWWTNSA-N icariin Chemical compound C1=CC(OC)=CC=C1C1=C(O[C@H]2[C@@H]([C@H](O)[C@@H](O)[C@H](C)O2)O)C(=O)C2=C(O)C=C(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)C(CC=C(C)C)=C2O1 TZJALUIVHRYQQB-XLRXWWTNSA-N 0.000 claims abstract description 22
- TZJALUIVHRYQQB-UHFFFAOYSA-N icariine Natural products C1=CC(OC)=CC=C1C1=C(OC2C(C(O)C(O)C(C)O2)O)C(=O)C2=C(O)C=C(OC3C(C(O)C(O)C(CO)O3)O)C(CC=C(C)C)=C2O1 TZJALUIVHRYQQB-UHFFFAOYSA-N 0.000 claims abstract description 22
- YKRGDOXKVOZESV-WRJNSLSBSA-N Paeoniflorin Chemical compound C([C@]12[C@H]3O[C@]4(O)C[C@](O3)([C@]1(C[C@@H]42)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)C)OC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-WRJNSLSBSA-N 0.000 claims abstract description 21
- 238000001228 spectrum Methods 0.000 claims abstract description 20
- DGFLRNOCLJGHLY-CYBMUJFWSA-N 5-O-methylvisamminol Natural products O(C)c1c2C(=O)C=C(C)Oc2cc2O[C@@H](C(O)(C)C)Cc12 DGFLRNOCLJGHLY-CYBMUJFWSA-N 0.000 claims abstract description 18
- 238000003908 quality control method Methods 0.000 claims abstract description 18
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 17
- 238000000985 reflectance spectrum Methods 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 7
- 238000004611 spectroscopical analysis Methods 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000009499 grossing Methods 0.000 claims description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 5
- 239000003814 drug Substances 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 241000903946 Clematidis Species 0.000 claims description 3
- 241000628997 Flos Species 0.000 claims description 3
- 241000283898 Ovis Species 0.000 claims description 3
- OFECPTGTEKSUPH-UHFFFAOYSA-N Visamminol Natural products CC1=CC(=O)c2cc3CC(Oc3cc2O1)C(C)(C)O OFECPTGTEKSUPH-UHFFFAOYSA-N 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 150000002338 glycosides Chemical class 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 241000196324 Embryophyta Species 0.000 claims description 2
- 238000010828 elution Methods 0.000 claims description 2
- 239000012362 glacial acetic acid Substances 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000010606 normalization Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 230000003595 spectral effect Effects 0.000 claims description 2
- 241000736199 Paeonia Species 0.000 claims 2
- 235000006484 Paeonia officinalis Nutrition 0.000 claims 2
- XSKZZVYURGCOGM-UHFFFAOYSA-N Ammiol Natural products O1C(CO)=CC(=O)C2=C1C(OC)=C1OC=CC1=C2OC XSKZZVYURGCOGM-UHFFFAOYSA-N 0.000 claims 1
- 238000005469 granulation Methods 0.000 claims 1
- 230000003179 granulation Effects 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000010183 spectrum analysis Methods 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 8
- 238000002329 infrared spectrum Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
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- 241001494479 Pecora Species 0.000 description 2
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- 230000000052 comparative effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- VYQNWZOUAUKGHI-UHFFFAOYSA-N monobenzone Chemical compound C1=CC(O)=CC=C1OCC1=CC=CC=C1 VYQNWZOUAUKGHI-UHFFFAOYSA-N 0.000 description 2
- 210000003205 muscle Anatomy 0.000 description 2
- 101150061025 rseP gene Proteins 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 208000006820 Arthralgia Diseases 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 235000019082 Osmanthus Nutrition 0.000 description 1
- 241000333181 Osmanthus Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000012361 intermediate testing Methods 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000003333 near-infrared imaging Methods 0.000 description 1
- YKRGDOXKVOZESV-UHFFFAOYSA-N paeoniflorin Natural products O1C(C)(C2(CC34)OC5C(C(O)C(O)C(CO)O5)O)CC3(O)OC1C24COC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000012372 quality testing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 206010039073 rheumatoid arthritis Diseases 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
Classifications
-
- 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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- 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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- 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
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention relates to a kind of numbness preparation and be dried the method for quick of intermediate multi objective, comprise the following steps: (1) measures numbness preparation and is dried moisture in intermediate standard substance, lactone glucoside of Radix Paeoniae, peoniflorin, 5 O methyl visamminol glycosides, icariin and the content of epimedin；(2) the infrared diffuse-reflectance spectrum of standard substance is gathered；(3) described spectrum is carried out pretreatment；(4) partial least square method is utilized to set up content prediction model；(5) gather the infrared diffuse-reflectance spectrum of testing sample and carry out pretreatment；(6) the pre-processed spectrum data of described testing sample are substituted into step (4) gained model, obtain the predictive value of respective components content respectively.Near-infrared spectral analysis technology is incorporated in the quality control of numbness preparation intermediate by the present invention, realize the quick mensuration to each quality control index content, shorten the detection time, save production cost, improve production efficiency and economic benefit, it is ensured that numbness tablet quality is safely, effectively.
Description
Technical field
The invention belongs near infrared detection technical field, be specifically related to a kind of numbness preparation and be dried the fast of intermediate multi objective
Speed detection method.
Background technology
Numbness preparation is by Herba Epimedii, the Radix Paeoniae Alba, Radix Rehmanniae, Radix Rehmanniae Preparata, Radix Dipsaci, Radix Aconiti Lateralis Preparata (Radix Aconiti Lateralis Preparata), Radix Angelicae Pubescentis, Rhizoma Drynariae, osmanthus
Branch, Radix Saposhnikoviae, Radix Clematidis, Spina Gleditsiae, Os Caprae seu Ovis, Rhizoma Cibotii (system), the Rhizoma Anemarrhenae, Herba Lycopodii, the compound recipe of Flos Carthami 17 taste drug matching
Preparation, its effect is invigorating the liver and kidney, bone and muscle strengthening, wind-damp dispelling, the meridian dredging, and for the numbness caused by deficiency of the liver and kindey, rheumatism resistance network, disease is seen
Muscle, arthralgia, locally enlargement, stiff deformity, joint stuffiness, soreness of the waist and knees, fear of cold is weak and rheumatoid arthritis is shown in
There is above-mentioned disease person etc..
Numbness preparation is extracted by modern extraction technique, through precipitate with ethanol, concentrate, be dried, the series of process means such as mixing obtain
The solid preparation made through preparations shaping technique to the solid intermediate being dried, including tablet, granule, capsule etc..?
It is the powder granular products obtained after drying that numbness preparation is dried intermediate.Dry run is the weight in numbness formulation manufacturing processes
Wanting process procedure, along with temperature rising, moisture content decline, the content of effective ingredient also occurs to change in the moment.Due to difference
The variation of the difference between the quality of medicinal material of batch and the key process parameter in dry run all can cause dry intermediate
Quality fluctuation, and then have influence on final product quality, therefore, in order to ensure Chinese medicine quality to greatest extent, need detection dry
The important quality index of dry intermediate.Presently, quality control relies primarily on experience and conventional mass analysis method (HPLC
Deng), time and effort consuming, analysis result is delayed, it is difficult to be widely used in production practices, therefore develops a kind of side that can quickly detect
Method, is dried intermediate quality for numbness preparation and controls have very much necessity and development prospect comprehensively.
Near-infrared spectrum analysis is the material information utilizing near infrared spectrum district to comprise, for material qualitative and quantitative analysis
A kind of analysis method, have analysis quickly, non-destructive and the advantage such as pollution-free.The near-infrared analysis time of sample is typically 30
Within Miao, and can multiple compositions or character to sample be measured simultaneously, compared with existing off-line analysis method, analysis time
More than 90% can be shortened.
It is dried in the quality testing of intermediate introducing near-infrared spectrum technique at numbness preparation, just can utilize near infrared light
It is quickly detected by spectral analysis technology advantage quick, lossless, without sample pretreatment, during feedback is dried intermediate in time
Active constituent content situation of change, so that it is guaranteed that end product quality.
Summary of the invention
It is an object of the invention to provide the near-infrared method for quick of a kind of numbness preparation intermediate multi objective, using should
Method can measure numbness preparation quickly and accurately and be dried moisture in intermediate, lactone glucoside of Radix Paeoniae content, paeoniflorin content, 5-O first
Base visamminol glycosides content, epimedin content and Icariin content, it is achieved to quickly commenting of numbness preparation intermediate quality
Valency.
Numbness preparation prescription of the present invention is particularly as follows: Radix Rehmanniae 20 parts, Radix Rehmanniae Preparata 20 parts, Radix Dipsaci 15 parts, Radix Aconiti Lateralis Preparata are (black suitable
Sheet) 15 parts, Radix Angelicae Pubescentis 10 parts, Rhizoma Drynariae 15 parts, Ramulus Cinnamomi 10 parts, Herba Epimedii 15 parts, the Radix Paeoniae Alba 12 parts, Radix Saposhnikoviae 10 parts, Radix Clematidis 15 parts,
Spina Gleditsiae 10 parts, Os Caprae seu Ovis 20 parts, Rhizoma Cibotii (system) 15 parts, the Rhizoma Anemarrhenae 15 parts, Herba Lycopodii 10 parts, 10 parts of Flos Carthami.
Intermediate of the present invention specifically refers to: Chinese medicine contained in above-mentioned prescription, as raw material, carries through water, after precipitate with ethanol,
It is concentrated into the thick paste that relative density is 1.27～1.30 (50 DEG C), mixes with adjuvant (including starch, dextrin), pelletize and be dried to containing
The water yield is 5%～6%, obtains midbody particle.
Specifically, the method that the present invention provides includes step in detail below:
(1) collect multiple numbness preparation and be dried the standard substance of intermediate, measure every Quality Control in each standard substance respectively and refer to
Target content；
Described quality control index includes: moisture, lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides, icariin
And epimedin；
(2) 4000～10000cm-1Sweep limits in, gather the infrared diffuse-reflectance spectrum of each standard substance；
(3) respectively the infrared diffuse-reflectance spectrum of each intermediate standard substance is carried out pretreatment；Described pretreatment particularly as follows:
Use first derivative to combine SG smoothing method and described spectrum is carried out pretreatment, use first derivative to combine Norris simultaneously and smooth
Method carries out pretreatment to described spectrum；
(4) use partial least square method (Partial least square regression, PLSR), set up step respectively
Suddenly moisture, lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides and the Icariin content and described that (1) measures
Order derivative combines the regression model between the spectroscopic data of SG smoothing method pretreatment gained, obtains numbness preparation and is dried intermediate
Middle moisture, lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides and icariin respective content prediction model；
Using partial least square method, the epimedin content that establishment step (1) measures is combined Norris with described first derivative
Regression model between the spectroscopic data of smoothing method pretreatment gained, obtains numbness preparation and is dried epimedin in intermediate
Content prediction model；
(5) take numbness preparation and be dried the testing sample of intermediate, use the method identical with step (2) to gather described to be measured
The infrared diffuse-reflectance spectrum of sample；
(6) use the first derivative identical with step (3) to be combined SG smoothing method the infrared of described testing sample is overflow instead
Penetrate spectrum and carry out pretreatment, described pretreatment the data obtained is substituted into step (4) described moisture, lactone glucoside of Radix Paeoniae, Radix Paeoniae respectively
Glycosides, 5-O methyl visamminol glycosides and Icariin content forecast model, obtain the predictive value of corresponding component content；
Use the first derivative identical with step (3) to be combined Norris smoothing method the infrared of described testing sample is overflow instead
Penetrate spectrum and carry out pretreatment, described pretreatment the data obtained is substituted into step (4) described epimedin content prediction model, to obtain final product
The predictive value of epimedin content.
In order to improve the accuracy of model prediction, simultaneously facilitating practical operation, step (1) the plurality of numbness preparation is dried
The number of the standard substance of intermediate is preferably 50～100, is taken respectively from different production batch.
Step (1) described moisture, lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides, icariin and court
The leaves of pulse plants is determined the content of C and is all used the method for this area routine to detect.
As a kind of preferred version, the assay method of step (1) described moisture is:
Precision weighs the sample that quality is 1g, 100～110 DEG C be dried 4～6h, move in exsiccator cool down 25～
35min, accurately weighed quality；It is dried 55～65min the most at the same temperature, moves to exsiccator cools down 25～35min, precision
Weighed quality, stops being dried to double dried difference difference less than 5mg；According to the difference meter of sample quality before and after being dried
Calculate moisture.
As a kind of preferred version, step (1) described lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides, excessive
The mensuration of sheep icariin and epimedin content uses high performance liquid chromatography, including following condition:
Chromatographic column is C18 post；
The A phase of flowing phase is 0.1% glacial acetic acid, and B phase is acetonitrile；Use gradient elution, particularly as follows: 0～15min, B phase is
15%；15～45min, B phase is 15%～19%；45～75min, B phase is 19%～32%；
Detection wavelength is 235～245nm；
Areas of peak normalization method is used to calculate lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides, excessive sheep respectively
Icariin and the content of epimedin.
Wherein, described high performance liquid chromatography also includes the pretreatment to sample, particularly as follows: take sample, and accurately weighed matter
Amount, adds Diluted Alcohol, supersound extraction 25～35min with 25ml/g, lets cool, and supplies weightlessness with Diluted Alcohol, crosses 0.45um filter membrane, i.e.
?.
The acquisition condition of the described infrared diffuse-reflectance spectrum of step of the present invention (2) includes: with air as reference, scanning times is
30～35 times, spectral resolution is 6～10cm-1.In order to improve the accuracy of model prediction, each sample at least gather 3 times red
Outer diffuse-reflectance spectrum, calculates averaged spectrum.
Owing to some irrelevant information and interference information can damage the performance of model, therefore step present in full spectrum
(3) need spectrum is carried out pretreatment.There is a large amount of known preprocessing procedures in this area, as without Pretreated spectra, SG
Smooth, first derivative+SG smooths, first derivative+Norris is smooth, second dervative+SG is smooth, second dervative+Norris smooths
Deng, the present invention by substantial amounts of experiment, preferably go out from a large amount of pretreatment modes for each quality control index specific pre-from
Reason mode, thus improve the predictive ability of model.
In order to accurately and comprehensively extract effective information as far as possible, simplified model and the predictive ability of raising model, this
Bright for each quality control index, concrete wave band and method to pretreatment have been carried out further preferably；Specifically:
Content prediction for moisture: extract 4500～7500cm-1In the range of spectroscopic data, use first derivative combine
Method smooth for SG carries out pretreatment；
Content prediction for lactone glucoside of Radix Paeoniae: extract 4500～7500cm-1In the range of spectroscopic data, use single order lead
Number combines method smooth for SG and carries out pretreatment；
Content prediction for peoniflorin: extract 4500～10000cm-1In the range of spectroscopic data, use first derivative
The method smooth in conjunction with SG carries out pretreatment；
Content prediction for 5-O methyl visamminol glycosides: extract 4000～10000cm-1In the range of spectroscopic data,
Use first derivative to combine method smooth for SG and carry out pretreatment；
Content prediction for icariin: extract 4300～4600cm-1, 5500～6100cm-1And 7500～
9400cm-1In the range of spectroscopic data, use first derivative to combine method smooth for SG and carry out pretreatment；
Content prediction for epimedin: extract 4500～10000cm-1In the range of spectroscopic data, use first derivative
The method smooth in conjunction with Norris carries out pretreatment.
Step of the present invention (4) described employing partial least square method sets up regression model, can use and known in the art have
The model of above-mentioned functions, software or instrument operate.As a kind of detailed description of the invention of the present invention, available existing closely
The software contained in infrared spectrometer (as purchased from the Bruker MATRIX-F of Brooker company of Germany) carries out offset minimum binary and returns
Return computing.
The method of the invention, can use calibration set correlation coefficient (Rc), checking collection correlation coefficient (Rp), calibration set mean square
Difference (Root mean square error in calibration, RMSEC), checking collection mean square deviation (Root mean square
Error in prediction, RMSEP), relative deviation (Relative standard errors of prediction,
Etc. RSEP) parameter investigates model performance.R is closer to the phase between 1 predictive value and the standard control methods analyst value representing model
Guan Xingyue is good；The size of RMSEC with RMSEP is relevant to sample chemical value, the two parameter the least closer to, then show model
Can be the best, it was predicted that precision is the highest；Requirement is controlled, when RSEP value is less than 20%, it is believed that institute's established model pre-according to actual mass
Survey precision in tolerance interval.
The quantitative model that the present invention provides can be verified by the following method: with checking collection sample to described quantitative model
Verify, gather the near infrared spectrum of intermediate to be measured, choose the wave band identical with calibration set sample spectra and pretreatment side
Method, imports built calibration model, it was predicted that go out the quality control index content of intermediate to be measured, the performance of checking model.
Near-infrared spectral analysis technology is incorporated in the quality control of numbness preparation intermediate by the present invention, it is achieved to each matter
The quick survey of control index (moisture, lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides, epimedin, icariin)
Fixed, shorten the detection time, save production cost, improve production efficiency and economic benefit, it is ensured that numbness tablet quality safely, have
Effect.
Accompanying drawing explanation
Fig. 1 is the near-infrared original absorbance spectrogram that numbness preparation is dried intermediate；
Fig. 2 is the comparison that numbness preparation is dried between actual value (i.e. measured value) and the predictive value of intermediate standard substance
Figure；
Fig. 3 is that the comparison that numbness preparation is dried between actual value (i.e. measured value) and the predictive value of intermediate testing sample is closed
System's figure.
Detailed description of the invention
Following example are used for illustrating the present invention, but are not limited to the scope of the present invention.
In following example, numbness sheet is dried midbody particle and is provided by Liaoning good nurse Pharmaceutical Co., Ltd；Closely
Infrared spectrometer model is Bruker MATRIX-F, purchased from Brooker company of Germany；High performance liquid chromatograph is U.S.'s Agilent
The 1100 of company；The reference substance of each quality control index composition is purchased from Man Site bio tech ltd, Chengdu.
Embodiment
Follow the steps below numbness preparation to be dried the multi objective of intermediate and quickly detect:
(1) collect the midbody particle of 88 batches of different dates of manufacture, be placed in dry sealing bag, there are 88 standards
Product；Each crucial quality control index is measured by traditional method, particularly as follows:
1) determination of moisture:
Precision weighs sample 1g in the flat bottle of dry constant weight, puts in baking oven and is dried 5h at 105 DEG C, moves in exsiccator
Cooling 30min, accurately weighed, then it is dried 1h at the temperature disclosed above, and cooling, weigh, to double difference less than 5mg, calculate
Moisture；
2) high performance liquid chromatography good fortune is used to measure lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides, Herba Epimedii
Glycosides and the content of epimedin:
A. sample pretreatment: take sample 1g, accurately weighed, precision adds the Diluted Alcohol of 25mL, supersound extraction 30min, lets cool,
Supply weightlessness with Diluted Alcohol, cross the filter membrane of 0.45um, to obtain final product；
B. liquid phase chromatogram condition: chromatographic column: Lichrospher C18 (4.6*250mm)；Flowing phase: A phase: 0.1% ice vinegar
Acid；B phase: acetonitrile；Gradient is arranged: 0-15min15%B；15-45min:15%-19%B；45-75min:19%-32%B；Inspection
Surveying wavelength 240nm, temperature is 25 DEG C, and flow velocity is 1mL/min, and sample size is 10 μ L；
(2) precision weighs sample 1g and puts in flat bottle, uses near infrared spectrometer to gather near-infrared diffuse-reflectance spectrum；Spectrum
Acquisition condition is: sweep limits is 4000～10000cm-1, with air as reference, scanning times is 32 times, and resolution is 8cm-1；3 spectrum of each sample collecting, calculate averaged spectrum；The original near infrared spectrum of standard substance is as shown in Figure 1；
(3) respectively the infrared diffuse-reflectance spectrum of each intermediate standard substance is carried out pretreatment；Described pretreatment particularly as follows:
Content prediction for moisture: extract 4500～7500cm-1In the range of spectroscopic data, use first derivative combine
Method smooth for SG carries out pretreatment；
Content prediction for lactone glucoside of Radix Paeoniae: extract 4500～7500cm-1In the range of spectroscopic data, use single order lead
Number combines method smooth for SG and carries out pretreatment；
Content prediction for peoniflorin: extract 4500～10000cm-1In the range of spectroscopic data, use first derivative
The method smooth in conjunction with SG carries out pretreatment；
Content prediction for 5-O methyl visamminol glycosides: extract 4000～10000cm-1In the range of spectroscopic data,
Use first derivative to combine method smooth for SG and carry out pretreatment；
Content prediction for icariin: extract 4300～4600cm-1, 5500～6100cm-1And 7500～
9400cm-1In the range of spectroscopic data, use first derivative to combine method smooth for SG and carry out pretreatment；
Content prediction for epimedin: extract 4500～10000cm-1In the range of spectroscopic data, use first derivative
The method smooth in conjunction with Norris carries out pretreatment；
(4) partial least square method is used, moisture that respectively establishment step (1) measures, lactone glucoside of Radix Paeoniae, peoniflorin, 5-O first
Base visamminol glycosides and Icariin content spectroscopic data to corresponding quality control index pretreatment gained described to step (3)
Between regression model, obtain numbness preparation and be dried moisture in intermediate, lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl Wei Sia meter
Alcohol glycosides and icariin respective content prediction model；
Using partial least square method, the epimedin content that establishment step (1) measures is described to step (3) to corresponding Quality Control
Regression model between the spectroscopic data of index pretreatment gained, obtains numbness preparation and is dried the content of epimedin in intermediate
Forecast model；
By standard substance respectively through measured value and the prediction utilizing above-mentioned forecast model gained of step (1) described method gained
Value compares, and the comparative result of part of standards product is as shown in Figure 2；
The forecast model partial parameters that each quality control index is corresponding refers to table 1；From table 1 it follows that the R of described model
Value is all higher than 0.85, RMSEC and RMSEP value is less and close to each other, illustrates that the stability of model is high, and generalization ability is good；
Table 1: the parameter of each quality control index content prediction model collects
(5) take numbness preparation and be dried 24 testing samples of intermediate；For each testing sample, use and step (2)
Identical method gathers the infrared diffuse-reflectance spectrum of described testing sample；
(6) for each testing sample, use the first derivative identical with step (3) to be combined SG smoothing method and treat described
The infrared diffuse-reflectance spectrum of test sample product carries out pretreatment, described pretreatment the data obtained is substituted into respectively step (4) described moisture,
Lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides and Icariin content forecast model, obtain corresponding composition and contain
The predictive value of amount；
Use the first derivative identical with step (3) to be combined Norris smoothing method the infrared of described testing sample is overflow instead
Penetrate spectrum and carry out pretreatment, described pretreatment the data obtained is substituted into step (4) described epimedin content prediction model, to obtain final product
The predictive value of epimedin content.
By testing sample respectively through step (1) described method gained measured value with utilize the pre-of above-mentioned forecast model gained
Measured value compares, and the comparative result of part testing sample is as shown in Figure 3；As can be seen from Figure 3 the content of 5 quality control indexs
Measured value is compared with predictive value, and without appreciable error, result is basically identical.
Although, used general explanation, detailed description of the invention and test, the present invention made detailed retouching
Stating, but on the basis of the present invention, can make some modifications or improvements it, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Scope.
Claims (10)
1. a numbness preparation is dried the method for quick of intermediate multi objective, it is characterised in that comprise the following steps:
(1) collect multiple numbness preparation and be dried the standard substance of intermediate, measure every quality control index in each standard substance respectively
Content；
Described quality control index includes: moisture, lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides, icariin and
Epimedin；
(2) 4000～10000cm-1Sweep limits in, gather the infrared diffuse-reflectance spectrum of each standard substance；
(3) respectively the infrared diffuse-reflectance spectrum of each intermediate standard substance is carried out pretreatment；Described pretreatment is particularly as follows: use
First derivative combines SG smoothing method and described spectrum carries out pretreatment, uses first derivative to combine Norris smoothing method simultaneously
Described spectrum is carried out pretreatment；
(4) partial least square method is used, moisture that respectively establishment step (1) measures, lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl dimension
This ammiol glycosides and Icariin content be combined with described first derivative SG smoothing method pretreatment gained spectroscopic data it
Between regression model, obtain numbness preparation and be dried moisture in intermediate, lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol
Glycosides and icariin respective content prediction model；
Using partial least square method, the epimedin content that establishment step (1) measures is combined Norris and smooths with described first derivative
Regression model between the spectroscopic data of method pretreatment gained, obtains numbness preparation and is dried the content of epimedin in intermediate
Forecast model；
(5) take numbness preparation and be dried the testing sample of intermediate, use the method identical with step (2) to gather described testing sample
Infrared diffuse-reflectance spectrum；
(6) use the first derivative identical with step (3) to be combined SG smoothing method the infrared of described testing sample is diffused
Spectrum carries out pretreatment, and described pretreatment the data obtained is substituted into step (4) described moisture, lactone glucoside of Radix Paeoniae, peoniflorin, 5-respectively
O methyl visamminol glycosides and Icariin content forecast model, obtain the predictive value of corresponding component content；
Use the first derivative identical with step (3) to be combined Norris smoothing method the infrared of described testing sample is diffused
Spectrum carries out pretreatment, described pretreatment the data obtained is substituted into step (4) described epimedin content prediction model, obtains towards the leaves of pulse plants
Determine the predictive value of C content.
Method the most according to claim 1, it is characterised in that described numbness preparation is dried intermediate with numbness preparation prescription
In contained Chinese medicine be raw material, carry through water, after precipitate with ethanol, be concentrated into the thick paste that relative density is 1.27～1.30, with auxiliary materials and mixing
After, it is 5%～6% that granulation is dried to water content, to obtain final product.
Method the most according to claim 2, it is characterised in that the prescription of described numbness preparation is particularly as follows: Radix Rehmanniae 20 parts, ripe
Radix Rehmanniae 20 parts, Radix Dipsaci 15 parts, Radix Aconiti Lateralis Preparata or Radix Aconiti Lateralis Preparata 15 parts, Radix Angelicae Pubescentis 10 parts, Rhizoma Drynariae 15 parts, Ramulus Cinnamomi 10 parts, Herba Epimedii 15 parts, white
Chinese herbaceous peony 12 parts, Radix Saposhnikoviae 10 parts, Radix Clematidis 15 parts, Spina Gleditsiae 10 parts, Os Caprae seu Ovis 20 parts, Rhizoma Cibotii processed 15 parts, the Rhizoma Anemarrhenae 15 parts, Herba Lycopodii 10
Part, 10 parts of Flos Carthami.
4. according to the method described in claims 1 to 3 any one, it is characterised in that during step (1) multiple numbness preparation is dried
The standard substance of mesosome are 50～100, are taken respectively from different production batch.
5. according to the method described in Claims 1 to 4 any one, it is characterised in that the mensuration of step (1) described moisture
Method is:
Precision weighs the sample that quality is 1g, is dried 4～6h at 100～110 DEG C, moves to cool down in exsiccator 25～35min, essence
Close weighed quality；It is dried 55～65min the most at the same temperature, moves to exsiccator cools down 25～35min, accurately weighed matter
Amount, stops being dried to double dried difference difference less than 5mg；Moisture is calculated according to the difference of sample quality before and after being dried
Content.
6. according to the method described in Claims 1 to 4 any one, it is characterised in that step (1) described lactone glucoside of Radix Paeoniae, Chinese herbaceous peony
The mensuration of medicine glycosides, 5-O methyl visamminol glycosides, icariin and epimedin content uses high performance liquid chromatography；
Preferably, described high performance liquid chromatography includes following condition:
Chromatographic column is C18 post；
The A phase of flowing phase is 0.1% glacial acetic acid, and B phase is acetonitrile；Use gradient elution, particularly as follows: 0～15min, B phase is
15%；15～45min, B phase is 15%～19%；45～75min, B phase is 19%～32%；
Detection wavelength is 235～245nm；
Areas of peak normalization method is used to calculate lactone glucoside of Radix Paeoniae, peoniflorin, 5-O methyl visamminol glycosides, icariin respectively
And the content of epimedin.
Method the most according to claim 6, it is characterised in that described high performance liquid chromatography also includes the pre-place to sample
Reason, particularly as follows: take sample, accurately weighed quality, add Diluted Alcohol, supersound extraction 25～35min with 25ml/g, let cool, with dilute
Weightlessness supplied by ethanol, crosses 0.45um filter membrane, to obtain final product.
8. according to the method described in claim 1～7 any one, it is characterised in that the described infrared diffuse-reflectance spectrum of step (2)
Acquisition condition include: with air as reference, scanning times is 30～35 times, and spectral resolution is 6～10cm-1。
Method the most according to claim 8, it is characterised in that each sample at least gathers 3 infrared diffuse-reflectance spectrum, meter
Calculate averaged spectrum.
10. according to the method described in claim 1～9 any one, it is characterised in that in described step (3):
Content prediction for moisture: extract 4500～7500cm-1In the range of spectroscopic data, use first derivative combine SG put down
Sliding method carries out pretreatment；
Content prediction for lactone glucoside of Radix Paeoniae: extract 4500～7500cm-1In the range of spectroscopic data, use first derivative knot
Close method smooth for SG and carry out pretreatment；
Content prediction for peoniflorin: extract 4500～10000cm-1In the range of spectroscopic data, use first derivative combine
Method smooth for SG carries out pretreatment；
Content prediction for 5-O methyl visamminol glycosides: extract 4000～10000cm-1In the range of spectroscopic data, use
First derivative combines method smooth for SG and carries out pretreatment；
Content prediction for icariin: extract 4300～4600cm-1, 5500～6100cm-1And 7500～9400cm-1
In the range of spectroscopic data, use first derivative to combine method smooth for SG and carry out pretreatment；
Content prediction for epimedin: extract 4500～10000cm-1In the range of spectroscopic data, use first derivative combine
Method smooth for Norris carries out pretreatment.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487395A (en) * | 2013-09-05 | 2014-01-01 | 浙江大学 | Quick multi-index detection method for Paris polyphylla medicinal materials |
| CN104316490A (en) * | 2014-11-10 | 2015-01-28 | 华润三九医药股份有限公司 | Method and application for rapidly detecting caulis spatholobi medicine material by using near infrared spectroscopy method |
| CN104359853A (en) * | 2014-11-10 | 2015-02-18 | 华润三九医药股份有限公司 | Method for quickly detecting ramulus uncariae cum uncis by utilizing near-infrared spectrometry and application of method |
| CN104833654A (en) * | 2015-05-13 | 2015-08-12 | 华润三九医药股份有限公司 | Method and application for rapidly detecting mother chrysanthemum medicinal materials by utilizing near infrared spectroscopy |
| CN105181637A (en) * | 2015-09-06 | 2015-12-23 | 正大青春宝药业有限公司 | Method for rapidly determining content of quality indexes of red ginseng by using near infrared diffuse reflection spectrum |
| CN105866064A (en) * | 2016-05-03 | 2016-08-17 | 哈尔滨珍宝制药有限公司 | Method for rapidly measuring content of five saponins in radix-notoginseng medicinal materials with near infrared spectroscopy method and application |
-
2016
- 2016-08-30 CN CN201610765242.9A patent/CN106248620A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487395A (en) * | 2013-09-05 | 2014-01-01 | 浙江大学 | Quick multi-index detection method for Paris polyphylla medicinal materials |
| CN104316490A (en) * | 2014-11-10 | 2015-01-28 | 华润三九医药股份有限公司 | Method and application for rapidly detecting caulis spatholobi medicine material by using near infrared spectroscopy method |
| CN104359853A (en) * | 2014-11-10 | 2015-02-18 | 华润三九医药股份有限公司 | Method for quickly detecting ramulus uncariae cum uncis by utilizing near-infrared spectrometry and application of method |
| CN104833654A (en) * | 2015-05-13 | 2015-08-12 | 华润三九医药股份有限公司 | Method and application for rapidly detecting mother chrysanthemum medicinal materials by utilizing near infrared spectroscopy |
| CN105181637A (en) * | 2015-09-06 | 2015-12-23 | 正大青春宝药业有限公司 | Method for rapidly determining content of quality indexes of red ginseng by using near infrared diffuse reflection spectrum |
| CN105866064A (en) * | 2016-05-03 | 2016-08-17 | 哈尔滨珍宝制药有限公司 | Method for rapidly measuring content of five saponins in radix-notoginseng medicinal materials with near infrared spectroscopy method and application |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645491A (en) * | 2016-12-28 | 2017-05-10 | 辽宁上药好护士药业（集团）有限公司 | Method for establishing fingerprint of lame impediment treating pills and method for identifying lame impediment treating pills by using fingerprint method |
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| CN109828059A (en) * | 2019-04-02 | 2019-05-31 | 成都中医药大学 | The detection method of Guizhi-Shoyao-Zhimu Decoction |
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