CN102973621B - A kind of three taste santal oral liquid and detection methods thereof - Google Patents
A kind of three taste santal oral liquid and detection methods thereof Download PDFInfo
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- OEYQBKYISMRWQB-UHFFFAOYSA-N Santal Chemical compound C=1C(OC)=CC(O)=C(C2=O)C=1OC=C2C1=CC=C(O)C(O)=C1 OEYQBKYISMRWQB-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 239000007788 liquid Substances 0.000 title claims abstract description 55
- 238000001514 detection method Methods 0.000 title claims abstract description 10
- 239000000341 volatile oil Substances 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 36
- 241000498779 Myristica Species 0.000 claims abstract description 29
- 235000009421 Myristica fragrans Nutrition 0.000 claims abstract description 29
- YQUVCSBJEUQKSH-UHFFFAOYSA-N 3,4-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 claims abstract description 28
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000001702 nutmeg Substances 0.000 claims abstract description 28
- 229940074391 gallic acid Drugs 0.000 claims abstract description 14
- 235000004515 gallic acid Nutrition 0.000 claims abstract description 14
- 238000003556 assay Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 90
- 239000000243 solution Substances 0.000 claims description 63
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 42
- OKKJLVBELUTLKV-UHFFFAOYSA-N methyl alcohol Substances OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- 238000012360 testing method Methods 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000002360 preparation method Methods 0.000 claims description 27
- 238000000605 extraction Methods 0.000 claims description 25
- 239000012467 final product Substances 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000284 extract Substances 0.000 claims description 18
- 239000013558 reference substance Substances 0.000 claims description 18
- 238000010992 reflux Methods 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 13
- 239000003921 oil Substances 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 6
- 239000007767 bonding agent Substances 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
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- 239000007924 injection Substances 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 238000004811 liquid chromatography Methods 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 6
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 6
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- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- FZRCKLPSHGTOAU-UHFFFAOYSA-N 6-amino-1,4-dimethylcyclohexa-2,4-diene-1-carbaldehyde Chemical compound CC1=CC(N)C(C)(C=O)C=C1 FZRCKLPSHGTOAU-UHFFFAOYSA-N 0.000 claims description 3
- DLMBWJZTIYLJQJ-UHFFFAOYSA-N OC=O.CCOC=O.CCCCCC Chemical compound OC=O.CCOC=O.CCCCCC DLMBWJZTIYLJQJ-UHFFFAOYSA-N 0.000 claims description 3
- WORJEOGGNQDSOE-UHFFFAOYSA-N chloroform;methanol Chemical compound OC.ClC(Cl)Cl WORJEOGGNQDSOE-UHFFFAOYSA-N 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000003814 drug Substances 0.000 abstract description 8
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- 235000012054 meals Nutrition 0.000 description 11
- 229920001213 Polysorbate 20 Polymers 0.000 description 10
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 10
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 10
- 238000003756 stirring Methods 0.000 description 9
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical class C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000004334 sorbic acid Substances 0.000 description 8
- 235000010199 sorbic acid Nutrition 0.000 description 8
- 229940075582 sorbic acid Drugs 0.000 description 8
- UEDUENGHJMELGK-HYDKPPNVSA-N Stevioside Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O UEDUENGHJMELGK-HYDKPPNVSA-N 0.000 description 6
- OHHNJQXIOPOJSC-UHFFFAOYSA-N stevioside Natural products CC1(CCCC2(C)C3(C)CCC4(CC3(CCC12C)CC4=C)OC5OC(CO)C(O)C(O)C5OC6OC(CO)C(O)C(O)C6O)C(=O)OC7OC(CO)C(O)C(O)C7O OHHNJQXIOPOJSC-UHFFFAOYSA-N 0.000 description 6
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- 206010000087 Abdominal pain upper Diseases 0.000 description 2
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- 230000000721 bacterilogical effect Effects 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical class OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000010411 cooking Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 208000029078 coronary artery disease Diseases 0.000 description 2
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- 239000004615 ingredient Substances 0.000 description 2
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- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- -1 oxybenzene ester Chemical class 0.000 description 2
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- 239000002904 solvent Substances 0.000 description 2
- DWNBOPVKNPVNQG-LURJTMIESA-N (2s)-4-hydroxy-2-(propylamino)butanoic acid Chemical compound CCCN[C@H](C(O)=O)CCO DWNBOPVKNPVNQG-LURJTMIESA-N 0.000 description 1
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 1
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 description 1
- 206010002383 Angina Pectoris Diseases 0.000 description 1
- 239000005711 Benzoic acid Chemical class 0.000 description 1
- 201000006306 Cor pulmonale Diseases 0.000 description 1
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 229920002307 Dextran Polymers 0.000 description 1
- 206010013954 Dysphoria Diseases 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 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 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Natural products OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- 208000004186 Pulmonary Heart Disease Diseases 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 238000000540 analysis of variance Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 1
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- FZWBNHMXJMCXLU-BLAUPYHCSA-N isomaltotriose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@@H](OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O)O1 FZWBNHMXJMCXLU-BLAUPYHCSA-N 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention relates to a kind of three taste santal oral liquid and detection methods thereof, described three taste santal oral liquids are by obtained after santal, nutmeg, fructus choerospondiatis three taste Chinese crude drug effective component extracting, and described detection method, comprises santal, nutmeg indentification by TLC; Assay comprises the assay of protocatechuic acid, gallic acid, and content assaying method is the mensuration of high performance liquid chromatography and volatile oil total amount.<!--1-->
Description
Technical field
The invention belongs to pharmaceutical field, be specifically related to a kind ofly there is heat-clearing effect to be particularly useful for clearing away heart-fire the preparation of three taste santal oral liquids of heat and method of quality control thereof.
Background technology
Three taste santal compounds are made up of santal, fructus choerospondiatis and nutmeg three taste medicinal material, and its function cures mainly as heat-clearing, and bushing is throbbed with fear for heart warmheartedness, the heart diseases such as dysphoria, as very remarkable in the curative effect such as coronary heart disease, pulmonary heart disease to treatment heart disease.Current three taste santal compounds have multiple formulations such as powder, capsule and granule, but the deficiency of existing preparation is: powder carries inconvenience, and easily the moisture absorption goes bad, and volatile ingredient can not be preserved for a long time; And hard capsule softgel shell dissolves slowly, cause drug effect slow; The easy moisture absorption of granule goes bad, and time more of a specified duration containing the storage of volatile-type composition, content easily declines.The advantage of oral liquid does not need disintegration, directly enters intestines and stomach, be beneficial to absorption, and bioavilability is good, is specially adapted to angiocardiopathy.Therefore, be necessary to develop a kind of three taste santal oral liquids.
Three taste santal oral liquids in the market continue to use classic method because of its preparation method, the difficult quality of its oral liquid controls, need to improve preparation technology for this reason, the oral liquid obtained is made to be not less than conventional art in effect, can control its quality simultaneously, be conducive to the Quality advance of product.
For effectively controlling the quality of product, we establish three taste santal oral liquid method of quality control, the method adopts thin-layered chromatography to differentiate santal, nutmeg, adopt high performance liquid chromatography to carry out assay to protocatechuic acid and gallic acid, the volatile oil of nutmeg and santal is measured.This method of quality control specificity, stability, accuracy are all better, can guarantee the safety and stability of product quality, effectively controlled.
Summary of the invention
The object of the present invention is to provide and a kind ofly there is heat-clearing effect to be particularly useful for clearing away heart-fire three taste santal oral liquid formulations of heat and new preparation method, a kind of detection method is provided simultaneously.
Three taste santal oral liquids of the present invention comprise following Chinese medicine material medicine:
Santal 100-300 part nutmeg 100-300 part fructus choerospondiatis 100-300 part
Preferred optimum formula consists of:
Santal 130 portions of nutmegs 130 portions of fructus choerospondiatis 130 parts
More than in composition, the weight of each taste medicine calculates with crude drug, if every 1 part in grams, above-mentioned formula composition can be made into 1000ml.
More than composition is by weight as proportioning, can increase by corresponding proportion when producing or reduce, as large-scale production can by kilogram in units of, or in units of ton; Small-scale production also can in units of milligram, the constant rate of the Chinese crude drug weight proportion of each composition.
In the present invention, fructus choerospondiatis is extracted can be that alcohol reflux extracts, and also can be seepage pressure effects.
Flavouring in the present invention includes but not limited to maltose, glucose, fructose, dextran, glycosides propylhomoserin, starch, sucrose, lactose, mannitol, stevioside etc., can be wherein one or several combinations.
The antiseptic that the present invention adds, includes but not limited to sorbic acid, benzoic acid, oxybenzene ester class etc., and can be wherein a kind of, also can be the combination of two kinds.
The present invention three taste santal oral liquid preparation process is as follows:
1) get fructus choerospondiatis appropriate, be ground into meal, take 100-300g, extract 2 times with 6 times amount 70-80% alcohol refluxs, filter, the dregs of a decoction are for subsequent use, reclaim ethanol and obtain liquid;
2) get santal and nutmeg appropriate, santal medicinal material wood shavings, ground nutmeg is broken into meal, respectively takes 100-300g, mixing, and with steam method refluxing extraction volatile oil, be separated volatile oil, sealing is preserved, and the dregs of a decoction are for subsequent use;
3) mixed by the dregs of a decoction of three taste medicinal materials, poach 1 time, filter, liquid hold over night, gets supernatant, concentrated, places room temperature, and 50-70% concentration of alcohol stirs alcohol precipitation, leaves standstill 24-48 hour, and filter, decompression filtrate recycling ethanol, obtains concentrate;
4) by fructus choerospondiatis alcohol extract with merges with alcohol precipitation concentrate, adding distil water is about 1000ml to volume, 4 DEG C refrigerate 48 hours.Room temperature bacteriological filtration plate suction filtration, it is 0.2% that filtrate adds sorbic acid to concentration, and after boiling 15 minutes, adding stevioside to concentration is 0.3%, boil 1 minute, the volatile oil of extraction and Tween-20 are stirred and evenly mixed with 1:5-1:6, slowly adds into the liquid (70 DEG C), strong agitation, 1000ml is settled to distilled water, filling, sterilizing, to obtain final product.
The preferred three taste santal oral liquid preparation processes of the present invention are as follows:
1) get fructus choerospondiatis appropriate, be ground into meal, take 130g, extract 2 times with 6 times amount 70-80% alcohol refluxs, filter, the dregs of a decoction are for subsequent use, reclaim ethanol and obtain liquid;
2) get santal and nutmeg appropriate, santal medicinal material wood shavings, ground nutmeg is broken into meal, respectively takes 130g, mixing, and with steam method refluxing extraction volatile oil 3h, be separated volatile oil, sealing is preserved, and the dregs of a decoction are for subsequent use;
3) mixed by the dregs of a decoction of three taste medicinal materials, 10 times amount poach 1 time, filter, liquid hold over night, gets supernatant, concentrated, places room temperature, and 60% concentration of alcohol stirs alcohol precipitation, leaves standstill 24 hours, and filter, decompression filtrate recycling ethanol, obtains concentrate;
4) by fructus choerospondiatis alcohol extract with merges with alcohol precipitation concentrate, adding distil water is about 1000ml to volume, 4 DEG C refrigerate 48 hours.Room temperature bacteriological filtration plate suction filtration, it is 0.2% that filtrate adds sorbic acid to concentration, and after boiling 15 minutes, adding stevioside to concentration is 0.3%, boil 1 minute, the volatile oil of extraction and Tween-20 are stirred and evenly mixed with 1:5-1:6, slowly adds into the liquid (70 DEG C), strong agitation, 1000ml is settled to distilled water, filling, sterilizing, to obtain final product.
Below in conjunction with testing, preparation method of the present invention is described:
1) santal, nutmeg volatile oil is drawn
Volatile oil is santal and myristicly mainly contains effective constituent, and we have investigated the oil pump capacity of different extraction time, and concrete grammar is that santal medicinal material is made wood shavings shape, ground nutmeg is broken into meal, carries out steam extraction, isolates volatile oil, in the dregs of a decoction and bottle, recirculation water stays for subsequent use, the results are shown in Table 1.
Oily result put forward by table 1 santal and nutmeg
From data in table, water vapor refluxing extraction volatile oil, reflux after 3 hours, oil mass no longer increases substantially, and therefore, return time 3 hours is optimum extraction time.
2) determination of dregs of a decoction extraction conditions
By three kinds of dregs of a decoction mixing poach, take paste-forming rate as Testing index, extract effective ingredient wherein further.Concrete technology condition positive quadraturing design test method draws.A-amount of water (multiple), B-poach time (hour), C-poach number of times carries out Three factors, three levels are investigated.In table 2.
Table 2 empirical factor table
Experimental result range analysis shows, factor A, B, C are A > B > C on the impact of paste-forming rate, the results of analysis of variance shows, amount of water and decocting time have significant to extraction result, extraction time is without significant, illustrate that affecting paste-forming rate principal element is solvent consumption, and extraction time impact is little.And suitably can shorten extraction time for economic consideration from production is and reduces extraction time, therefore produce above employing 10 times of water gagings, 1 decoction and be advisable for 2 hours.
3) selection of alcohol precipitation concentration
Poach concentrate carries out alcohol precipitation with 50%, 60%, 70% ethanol respectively, makes oral liquid, and place and observe its situation of change, three batches, each alcohol precipitation concentration sample, it the results are shown in following table 3.
The selection of table 3 alcohol precipitation concentration
"-" represents that clarification " ± " represents that slightly muddy "+" represents muddy
Can be drawn by above result, alcohol precipitation concentration be the oral liquid of 50% through placing after certain hour, slightly precipitate, alcohol precipitation concentration be 60%, 70% oral liquid still clarify through placing, alcohol precipitation concentration of the present invention selects 60%.
4) solubilizer
In order to ensure the clarity of oral liquid, stability etc. meet the requirements, and test by the screening to non-ionic surfactants such as Tween-20, Tween-60, Tween-80s, determine Tween-20 and volatile oil is miscible adds best results in oral liquid.And relevant theoretical according to materialization, Tween-20 content in liquid reaches its critical micelle concentration (CMC) just can play solubilization.The present invention adopts the CMC of Tween-20 in By Means of Electrical Conductivity oral liquid for this reason.Its principle by: Tween-20 with carried volatile oil and be combined and form critical micelle concentration (CMC), learn optimum proportioning by the catastrophe point of conductivity value and surfactant materials concentration relationship curve.
Oral liquid 1000ml(is prepared not containing volatile oil by technique of the present invention), be divided into 10 equal portions.Extracted volatile oil is divided into 10 equal portions, make 1:0,1:1,1:2,1:3,1:4,1:5,1:6,1:7,1:8(with Tween-20 respectively and all do not add sorbic acid) and 1:0(add 0.2% sorbic acid), after stirring, join in 100ml oral liquid sample respectively, then on DDS-11A type conductivity meter, measure conductivity respectively, the results are shown in Table 4.
Result shows that catastrophe point is between 1:5-1:6, and for guaranteeing clarity of oral liquid of the present invention, selective volatilization oil of the present invention is 1:6 with Tween-20 proportioning.
Table 4 Tween-20 consumption and oral liquid electric conductivity value relation
The present invention also provides the detection method of the present invention three taste santal oral liquid, and described detection method comprises following major part:
1) santal, nutmeg in pharmaceutical preparation of the present invention are differentiated;
2) gallic acid of fructus choerospondiatis, the content of protocatechuic acid in pharmaceutical preparation of the present invention are measured;
3) content of the volatile oil in santal, nutmeg in pharmaceutical preparation of the present invention is measured.
Above-mentioned part concrete operations are as follows:
1) this product 100ml is got, water-bath is transferred in separating funnel after being concentrated into thick paste, by extracted with diethyl ether to the complete layering of solution, is poured in evaporating dish by the solution after extraction and treats that solution evaporates into without ether taste completely, add chloroform 5ml more wherein and make dissolving, as need testing solution.Separately get nutmeg control medicinal material 10g, boiling 1h, filters while hot, and filtrate is concentrated into thick paste, is made in the same way of control medicinal material solution.Draw each 15 μ l of above-mentioned two kinds of solution, put respectively in same with sodium carboxymethyl cellulose be bonding agent silica gel g thin-layer plate on, with chloroform-methyl alcohol (95:5) for developping agent, launch, take out, dry, spray with sulfuric acid-methyl alcohol (1:1) solution, dry 5 minutes under 105 degrees Celsius, inspect under putting uviol lamp (365nm).In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
2) get this product 30ml, extract at twice with ether 20ml, merge ether solution, be vaporized ether to 2ml, as need testing solution; Separately get santal control medicinal material, extract volatile oil by determination of volatile oil Division A League Matches of French Football method (Chinese Pharmacopoeia version annex XD in 2010), add diethyl ether and make the solution of 1ml containing 0.1ml, medicinal material solution in contrast.Test according to thin-layered chromatography (Chinese Pharmacopoeia version annex VIB in 2010), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same with sodium carboxymethyl cellulose be bonding agent silica gel g thin-layer plate on, with sherwood oil (60 ~ 90 DEG C)-normal hexane-ethyl formate-formic acid (1:3:1.5:0.1) for developping agent, launch, take out, dry, spray, with paradime thylaminobenzaldehyde solution, is dried 5 minutes at 80 ~ 90 DEG C.In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the spot of aobvious same color.
3) assay of the present invention:
The mensuration of a protocatechuic acid
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Methanol-water (containing 2.5% acetic acid) (10:90) is mobile phase, and determined wavelength is 260nm.Number of theoretical plate calculates should be not less than 2500 by protocatechuic acid peak.
The preparation of reference substance solution gets protocatechuic acid reference substance in right amount, accurately weighed, adds 70% ethanol and dissolves, and makes the solution of every 1ml containing 0.1mg, to obtain final product.
The preparation of need testing solution accurately measures this product 10.00ml, and in evaporating dish, water bath method, residue adds 70% ethanol and dissolves and be transferred in 10ml measuring bottle, adds 70% ethanol to scale, shakes up, and filters, to obtain final product with miillpore filter (0.45 μm).
Determination method respectively precision measures reference substance and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
This product is often propped up containing fructus choerospondiatis with protocatechuic acid (C
7h
6o
4), must not 0.09mg be less than.
The mensuration of b gallic acid
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Methyl alcohol-0.2% aqueous formic acid (6:94) is mobile phase, and determined wavelength is 270nm.Number of theoretical plate calculates should be not less than 3000 by gallic acid peak.
The preparation of reference substance solution gets gallic acid reference substance in right amount, accurately weighed, adds 50% methyl alcohol and dissolves, and makes the solution of every 1ml containing 0.1mg, to obtain final product.
The preparation of need testing solution accurately measures this product 10.00ml, and in evaporating dish, water bath method, residue adds 50% methyl alcohol and dissolves and be transferred in 10ml measuring bottle, adds methyl alcohol to scale, shakes up, and filters, to obtain final product with miillpore filter (0.45 μm).
Determination method respectively precision measures reference substance and each 5 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
This product is often propped up containing fructus choerospondiatis with gallic acid (C
7h
8o
6), must not 0.07mg be less than.
4) determination of volatile oil:
Get three taste santal sample 100ml(to be about equivalent to containing volatile oil 0.5 ~ 1.0ml), put in flask, add water appropriate and beaded glass number, after jolting mixing, connects volatile oil determination apparatus and reflux condensing tube.Autocondensation pipe upper end adds water and makes to be full of the scale part of volatile oil determination apparatus, and when overflow enters flask till.Put in electric jacket or by other proper method and be slowly heated to boil, and keep micro-and boil about 5 hours, to analyzer, oil mass no longer increases, stop heating, place a moment, open the piston of analyzer lower end, water is slowly released, to 5mm place above oil reservoir upper end arrival scale 0 line.Place more than 1 hour, then open piston and make oil reservoir drop to its upper end just and scale.Line is concordant, reads volatilization oil mass, and calculates the content (%) of volatile oil in test sample.
This product is often propped up and must not be less than 0.05ml containing volatile oil.
The invention provides santal, myristic indentification by TLC, have selected effective constituent protocatechuic acid in fructus choerospondiatis and gallic acid as assay index, establish volatile oil standard in the content assaying method of three taste santals and three taste santals; Have passed through repeated experiment, confirmation method is easy, repeatability is good, can as the quality control index of three taste santal oral liquids.
Three taste santal oral liquids of the present invention can determine usage and dosage according to the concrete condition of patient in use.
Three taste santal oral liquids of the present invention, have in promoting the circulation of qi temperature, the result for the treatment of of appetizing pain relieving, for cold obstruction causing qi stagnation, and pectoralgia, stomachache, stomachache food is few; Coronary heart disease, angina pectoris.
Following examples are for further illustrating the feasibility of three taste santal oral liquid preparation technologies, and three taste santal oral liquids of this explained hereafter are stable and controllable for quality.
Embodiment
The preparation method of specific embodiment 1: three taste santal oral liquid
Prescription: santal 130g nutmeg 130g fructus choerospondiatis 130g
Method for making:
1, medicinal material pre-treatment: santal electric planer is dug into wood shavings shape, then pulverizes with comminutor, and nutmeg comminutor is pulverized (when noting pulverizing, machine temperature can not be too high, to prevent the loss of volatile oil), and the comminutor of fructus choerospondiatis is pulverized.
2, the preparation of fructus choerospondiatis alcohol extract: get fructus choerospondiatis meal 130g 70%-80% alcohol reflux and extract twice, first time 2.0h, second time 2.0h, filter, the dregs of a decoction are for subsequent use, reclaim ethanol, obtain concentrated medicament.
3, the extraction of santal and nutmeg volatile oil: santal mixes with each 130g meal of nutmeg, with steam method refluxing extraction volatile oil, separates volatile oil, sealing is preserved, and the dregs of a decoction are for subsequent use.
4, mix the preparation of medicinal material water cooking liquid: mixed by the dregs of a decoction of three taste medicinal materials, poach, filter, merge liquid, hold over night, gets supernatant, concentrated, leaves standstill room temperature, alcohol precipitation (regulating the concentration 60% of alcohol precipitation) stirs and leaves standstill 24 hours, and filter, decompression filtrate recycling ethanol, obtains concentrate.
5, prepare burden: by fructus choerospondiatis alcohol extract with merges with poach concentrate, adding distil water is about 800ml to volume, 4 DEG C refrigerate 48 hours.Room temperature board and frame machine suction filtration, it is 0.2% that filtrate adds sorbic acid to concentration, after boiling 15 minutes, adding stevioside to concentration is 0.3%, boil 1 minute, cool to room temperature, the volatile oil of extraction and polysorbas20 are stirred and evenly mixed with 1:6, slowly add into the liquid, stir, be settled to 1000ml with distilled water, filling, sterilizing, to obtain final product.
The preparation method of specific embodiment 2: three taste santal oral liquid
Prescription: santal 130g nutmeg 130g fructus choerospondiatis 130g
Method for making:
1, medicinal material pre-treatment: santal electric planer is dug into wood shavings shape, then pulverizes with comminutor, and nutmeg comminutor is pulverized (when noting pulverizing, machine temperature can not be too high, to prevent the loss of volatile oil), and fructus choerospondiatis comminutor is pulverized.
2, the preparation of fructus choerospondiatis alcohol extract: get fructus choerospondiatis meal 130g 70%-80% ethanol percolation, soaks 24h, and with the speed of 3ml/kg/min slowly diacolation, collect percolate, reclaim ethanol, being concentrated into proportion is 1.15(60 DEG C), the dregs of a decoction are for subsequent use.
3, the extraction of santal and nutmeg volatile oil: santal mixes with each 130g meal of nutmeg, with steam method refluxing extraction volatile oil, separates volatile oil, sealing is preserved, and the dregs of a decoction are for subsequent use.
4, mix the preparation of medicinal material water cooking liquid: mixed by the dregs of a decoction of three taste medicinal materials, poach, filter, merge liquid, hold over night, gets supernatant, concentrated, leaves standstill room temperature, and alcohol precipitation stirs and leaves standstill 24 hours, and filter, decompression filtrate recycling ethanol, obtains poach concentrate.
5, prepare burden: by fructus choerospondiatis alcohol extract with merges with poach concentrate, adding distil water is about 800ml to volume, 4 degrees Celsius refrigerate 48 hours.Dosing is through centrifuge, and it is 0.2% that the filtrate after centrifugal adds sorbic acid to concentration, after boiling 15 minutes, adding stevioside to concentration is 0.3%, boils 1 minute, cooling room temperature, the volatile oil of extraction and polysorbas20 are stirred and evenly mixed with 1:6, adds into the liquid, stir, 1000ml is settled to distilled water, filling, sterilizing, to obtain final product.
By the following examples, more detailed explanation is done to detection method of the present invention, but not as restriction.
Embodiment 3: get fructus choerospondiatis meal 70% alcohol reflux and extract twice, filter, the dregs of a decoction are for subsequent use, reclaim ethanol and obtain liquid; Santal mixes with each meal of nutmeg, with steam method refluxing extraction volatile oil, separates volatile oil, and sealing is preserved, and the dregs of a decoction are for subsequent use.Mixed by the dregs of a decoction, poach, filter, merge liquid, hold over night, gets supernatant, concentrated, leaves standstill room temperature, and alcohol precipitation (regulating the concentration 60% of alcohol precipitation) stirs, and leave standstill 24 hours, filter, decompression filtrate recycling ethanol, obtains poach concentrate.By fructus choerospondiatis alcohol extract with merges with poach concentrate, adding distil water is about 800ml to volume, 4 DEG C refrigerate 48 hours.Room temperature board and frame machine filters, and it is 0.2% that filtrate adds sorbic acid to concentration, after boiling 15 minutes, adding stevioside to concentration is 0.3%, boils 1 minute, cooling room temperature, the volatile oil of extraction and polysorbas20 are stirred and evenly mixed with 1:6, adds into the liquid, stir, 1000ml is settled to distilled water, filling, sterilizing, to obtain final product.
Prepare with method, obtained medicine amounts to 6 batches altogether, is respectively: 20120809,20120827,20120918,20120926,20121011,20121029. in batches
Above 6 batch detection methods comprise following methods:
1) this product 100ml is got, water-bath is transferred in separating funnel after being concentrated into thick paste, by extracted with diethyl ether to the complete layering of solution, is poured in evaporating dish by the solution after extraction and treats that solution evaporates into without ether taste completely, add chloroform 5ml more wherein and make dissolving, as need testing solution.Separately get nutmeg control medicinal material 10g, boiling 1h, filters while hot, and filtrate is concentrated into thick paste, is made in the same way of control medicinal material solution.Test according to thin-layered chromatography (Chinese Pharmacopoeia version annex VIB in 2010), draw each 15 μ l of above-mentioned two kinds of solution, put respectively in same with sodium carboxymethyl cellulose be bonding agent silica gel g thin-layer plate on, with chloroform-methyl alcohol (95:5) for developping agent, launch, take out, dry, spray, with sulfuric acid-methyl alcohol (1:1) solution, is dried 5 minutes, is inspected under putting uviol lamp (365nm) under 105 degrees Celsius.In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color.
2) get this product 30ml, extract at twice with ether 20ml, merge ether solution, be vaporized ether to 2ml, as need testing solution.Separately get santal control medicinal material, extract volatile oil by determination of volatile oil Division A League Matches of French Football method (Chinese Pharmacopoeia version annex XD in 2010), add diethyl ether and make the solution of 1ml containing 0.1ml, medicinal material solution in contrast.Test according to thin-layered chromatography (Chinese Pharmacopoeia version annex VIB in 2010), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same with sodium carboxymethyl cellulose be bonding agent silica gel g thin-layer plate on, with sherwood oil (60 ~ 90 DEG C)-normal hexane-ethyl formate-formic acid (1:3:1.5:0.1) for developping agent, launch, take out, dry, spray, with paradime thylaminobenzaldehyde solution, is dried 5 minutes at 80 ~ 90 DEG C.In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the spot of aobvious same color.
Assay of the present invention is one or both of following method:
Measure according to high performance liquid chromatography (Chinese Pharmacopoeia version annex VID in 2010).
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Methanol-water (containing 2.5% acetic acid) (10:90) is mobile phase, and determined wavelength is 260nm.Number of theoretical plate calculates should be not less than 2500 by protocatechuic acid peak.
The preparation of reference substance solution gets protocatechuic acid reference substance in right amount, accurately weighed, adds 70% ethanol and dissolves, and makes the solution of every 1ml containing 0.1mg, to obtain final product.
The preparation of need testing solution accurately measures this product 10.00ml, and in evaporating dish, water bath method, residue adds 70% ethanol and dissolves and be transferred in 10ml measuring bottle, adds 70% ethanol to scale, shakes up, and filters, to obtain final product with miillpore filter (0.45 μm).
Determination method respectively precision measures reference substance and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
This product is often propped up containing fructus choerospondiatis with protocatechuic acid (C
7h
6o
4), must not 0.09mg be less than.
2) measure according to high performance liquid chromatography (Chinese Pharmacopoeia version annex VID in 2010).
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filling agent; Methyl alcohol-0.2% aqueous formic acid (6:94) is mobile phase, and determined wavelength is 270nm.Number of theoretical plate calculates should be not less than 3000 by gallic acid peak.
The preparation of reference substance solution gets gallic acid reference substance in right amount, accurately weighed, adds 50% methyl alcohol and dissolves, and makes the solution of every 1ml containing 0.1mg, to obtain final product.
The preparation of need testing solution accurately measures this product 10.00ml, and in evaporating dish, water bath method, residue adds 50% methyl alcohol and dissolves and be transferred in 10ml measuring bottle, adds methyl alcohol to scale, shakes up, and filters, to obtain final product with miillpore filter (0.45 μm).
Determination method respectively precision measures reference substance and each 5 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
This product is often propped up containing fructus choerospondiatis with gallic acid (C
7h
8o
6), must not 0.07mg be less than.
This product is often propped up and must not be less than 0.05ml containing volatile oil.Drug test the results are shown in Table 5:
The assay of table 56 batch three taste santal oral liquids
Claims (1)
1. a detection method for three taste santal oral liquids, step is as follows:
A) nutmeg indentification by TLC gets three taste santal oral liquid 100ml, water-bath is transferred in separating funnel after being concentrated into thick paste, by extracted with diethyl ether to the complete layering of solution, solution after extraction is poured in evaporating dish and treats that solution evaporates into without ether taste completely, add chloroform 5ml more wherein and make dissolving, as need testing solution, separately get nutmeg control medicinal material 10g, boiling 1h, filter while hot, filtrate is concentrated into thick paste, be made in the same way of control medicinal material solution, draw each 15 μ l of above-mentioned two kinds of solution, put respectively in same with sodium carboxymethyl cellulose be bonding agent silica gel g thin-layer plate on, with chloroform-methyl alcohol: 95:5 for developping agent, launch, take out, dry, spray is with the solution of sulfuric acid-methyl alcohol=1:1, dry 5 minutes under 105 degrees Celsius, inspect under putting 365nm uviol lamp, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the fluorescence spot of aobvious same color,
B) santal indentification by TLC gets three taste santal oral liquid 30ml, extracts at twice with ether 20ml, merges ether solution, is vaporized ether to 2ml, as need testing solution, separately get santal control medicinal material, volatile oil is extracted by Chinese Pharmacopoeia version annex XD determination of volatile oil Division A League Matches of French Football method in 2010, add diethyl ether and make the solution of 1ml containing 0.1ml, medicinal material solution in contrast, according to Chinese Pharmacopoeia version annex VIB thin-layered chromatography test in 2010, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same with sodium carboxymethyl cellulose be bonding agent silica gel g thin-layer plate on, 60 ~ 90 DEG C, with sherwood oil-normal hexane-ethyl formate-formic acid=1:3:1.5:0.1 for developping agent, launch, take out, dry, spray is with paradime thylaminobenzaldehyde solution, dry 5 minutes at 80 ~ 90 DEG C, in test sample chromatogram, on the position corresponding to control medicinal material chromatogram, the spot of aobvious same color,
C) assay of protocatechuic acid
Be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol: water=10:90 is mobile phase, determined wavelength is 260nm, and number of theoretical plate calculates should be not less than 2500 by protocatechuic acid peak, and wherein said water is containing 2.5% acetic acid;
The preparation of reference substance solution gets protocatechuic acid reference substance in right amount, accurately weighed, adds 70% ethanol and dissolves, and makes the solution of every 1ml containing 0.1mg, to obtain final product;
The preparation of need testing solution accurately measures three taste santal oral liquid 10.00ml, in evaporating dish, and water bath method, residue adds 70% ethanol and dissolves and be transferred in 10ml measuring bottle, adds 70% ethanol to scale, shakes up, and filters, to obtain final product with 0.45 μm of miillpore filter;
Determination method respectively precision measures reference substance and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product;
D) assay of gallic acid
Be filling agent with octadecylsilane chemically bonded silica; Methyl alcohol: 0.2% aqueous formic acid=6:94 is mobile phase, determined wavelength is 270nm, and number of theoretical plate calculates should be not less than 3000 by gallic acid peak;
The preparation of reference substance solution gets gallic acid reference substance in right amount, accurately weighed, adds 50% methyl alcohol and dissolves, and makes the solution of every 1ml containing 0.1mg, to obtain final product;
The preparation of need testing solution accurately measures three taste santal oral liquid 10.00ml, in evaporating dish, and water bath method, residue adds 50% methyl alcohol and dissolves and be transferred in 10ml measuring bottle, adds methyl alcohol to scale, shakes up, and filters, to obtain final product with 0.45 μm of miillpore filter;
Determination method respectively precision measures reference substance and each 5 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product;
E) assay of volatile oil
Get three taste santal oral liquid 100ml, put in flask, add water appropriate and beaded glass number, after jolting mixing, connect volatile oil determination apparatus and reflux condensing tube, autocondensation pipe upper end adds water and makes to be full of the scale part of volatile oil determination apparatus, and overflow when entering flask till, put in electric jacket or by other proper method and be slowly heated to boil, and keep micro-and boil 5 hours, to analyzer, oil mass no longer increases, stop heating, place a moment, open the piston of analyzer lower end, water is slowly released, to 5mm place above oil reservoir upper end arrival scale 0 line, place more than 1 hour, opening piston again makes oil reservoir drop to its upper end just and scale, line is concordant, read volatilization oil mass, and calculate the content of volatile oil in test sample.
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| CN102507840A (en) * | 2011-11-07 | 2012-06-20 | 山东阿如拉药物研究开发有限公司 | Sanwei sandalwood granule and quality control method of preparation thereof |
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Address after: 336000 Yuanzhou pharmaceutical industry park, Jiangxi, Yichun Co-patentee after: Jiangxi Jinshuibao Pharmaceutical Co.,Ltd. Patentee after: JIANGXI JIMINKEXIN PHARMACEUTICAL Co.,Ltd. Address before: 336000 pharmaceutical industry park, Yuanzhou District, Jiangxi, Yichun Co-patentee before: JIANGXI JIMINKEXIN JINSHUIBAO PHARMACEUTICAL Co.,Ltd. Patentee before: JIANGXI JIMINKEXIN PHARMACEUTICAL Co.,Ltd. |
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Application publication date: 20130320 Assignee: JIANGXI JIMIN KEXIN MEDICINE Co.,Ltd. Assignor: JIANGXI JIMINKEXIN PHARMACEUTICAL Co.,Ltd. Contract record no.: X2023980053140 Denomination of invention: A Three Flavored Sandalwood Oral Liquid and Its Detection Method Granted publication date: 20160127 License type: Common License Record date: 20231219 |