CN101167909B - Content determination method of haw and corium stomachium galli preparation - Google Patents
Content determination method of haw and corium stomachium galli preparation Download PDFInfo
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- CN101167909B CN101167909B CN2007100663616A CN200710066361A CN101167909B CN 101167909 B CN101167909 B CN 101167909B CN 2007100663616 A CN2007100663616 A CN 2007100663616A CN 200710066361 A CN200710066361 A CN 200710066361A CN 101167909 B CN101167909 B CN 101167909B
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 135
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 230000007935 neutral effect Effects 0.000 claims abstract description 17
- 239000011347 resin Substances 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 239000000284 extract Substances 0.000 claims abstract description 15
- 239000003814 drug Substances 0.000 claims abstract description 12
- 239000003480 eluent Substances 0.000 claims abstract description 8
- 238000012360 testing method Methods 0.000 claims description 29
- KFFCKOBAHMGTMW-LGQRSHAYSA-N Forsythin Chemical compound C1=C(OC)C(OC)=CC=C1[C@H]1[C@@H](CO[C@@H]2C=3C=C(OC)C(O[C@H]4[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O4)O)=CC=3)[C@@H]2CO1 KFFCKOBAHMGTMW-LGQRSHAYSA-N 0.000 claims description 18
- 239000000706 filtrate Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000013558 reference substance Substances 0.000 claims description 14
- 241001092040 Crataegus Species 0.000 claims description 11
- 235000009917 Crataegus X brevipes Nutrition 0.000 claims description 11
- 235000013204 Crataegus X haemacarpa Nutrition 0.000 claims description 11
- 235000009685 Crataegus X maligna Nutrition 0.000 claims description 11
- 235000009444 Crataegus X rubrocarnea Nutrition 0.000 claims description 11
- 235000009486 Crataegus bullatus Nutrition 0.000 claims description 11
- 235000017181 Crataegus chrysocarpa Nutrition 0.000 claims description 11
- 235000009682 Crataegus limnophila Nutrition 0.000 claims description 11
- 235000004423 Crataegus monogyna Nutrition 0.000 claims description 11
- 235000002313 Crataegus paludosa Nutrition 0.000 claims description 11
- 235000009840 Crataegus x incaedua Nutrition 0.000 claims description 11
- 239000002775 capsule Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 241000576429 Forsythia suspensa Species 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 5
- 235000011305 Capsella bursa pastoris Nutrition 0.000 claims description 4
- 240000008867 Capsella bursa-pastoris Species 0.000 claims description 4
- 241000931705 Cicada Species 0.000 claims description 4
- 241000287828 Gallus gallus Species 0.000 claims description 4
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 4
- 210000004317 gizzard Anatomy 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 16
- 229940079593 drug Drugs 0.000 abstract description 8
- 230000001476 alcoholic effect Effects 0.000 abstract description 5
- 235000019441 ethanol Nutrition 0.000 abstract 2
- 229960004756 ethanol Drugs 0.000 abstract 2
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- 238000010971 suitability test Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 51
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 32
- 239000000463 material Substances 0.000 description 15
- 239000012535 impurity Substances 0.000 description 10
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- 238000003556 assay Methods 0.000 description 7
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- 239000000741 silica gel Substances 0.000 description 6
- 229910002027 silica gel Inorganic materials 0.000 description 6
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- 238000004587 chromatography analysis Methods 0.000 description 5
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- 238000011003 system suitability test Methods 0.000 description 4
- 238000004440 column chromatography Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000012907 honey Nutrition 0.000 description 3
- 210000000952 spleen Anatomy 0.000 description 3
- 210000002784 stomach Anatomy 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
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- 238000001035 drying Methods 0.000 description 2
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- 238000011049 filling Methods 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
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- 238000012546 transfer Methods 0.000 description 2
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 1
- 206010000060 Abdominal distension Diseases 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 208000006096 Attention Deficit Disorder with Hyperactivity Diseases 0.000 description 1
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- 208000015817 Infant Nutrition disease Diseases 0.000 description 1
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- 229920002472 Starch Polymers 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
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- 239000007791 liquid phase Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000003808 methanol extraction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000008194 pharmaceutical composition Substances 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 230000003285 pharmacodynamic effect Effects 0.000 description 1
- 239000004302 potassium sorbate Substances 0.000 description 1
- 229940069338 potassium sorbate Drugs 0.000 description 1
- 235000010241 potassium sorbate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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Abstract
The invention relates to a content measuring method of a Chinese patent drug. The steps of the invention are that the chromatographic condition and the systematical employment and suitability test are the first step. The preparation of the solution for comparison is the second step of the invention. 3. After extracting by methyl alcohol, the extract solution of the preparation specimen is concentrated to the low alcoholic solution or the alcoholic-free solution. 4. After the purge process 3, the concentration solution of the extract solution is transferred to the macroreticular resin of a neutral alumina pole, wherein the lower portion is neutral alumina, and the upper portion is pre-treated macroreticular resin. The upper portion and the lower portion are washed by water and a grain alcohol solution of 10-25% sequentially, then the pole is eluted by the grain alcohol solution of 50-95%, and the eluent is collected and evaporated to dryness, further the residue is dissolved and has the constant volume and the filtration. The sequent filtration solution is achieved as the specimen solution. 5. According to the measuration, the solution for comparison of 10 mul and the specimen solution of 20 mul are precisely extracted separately, and the liquid chromatograph is injected, after measuring, the aim is achieved.
Description
Technical field
The present invention relates to a kind of content assaying method of Chinese patent drug.
Background technology
Chinese patent application numbers 200410034161.9 discloses " medicine that a kind of strengthening the spleen and stomach, long-pendingization that disappear stagnate ", this invention relate to a kind of with natural plants, animal drug be main medicinal ingredient have that strengthening the spleen and stomach, long-pendingization that disappear are stagnant, the pharmaceutical composition of intelligence promoting and tranquilization effect.Be the medicament of making by the following weight proportion raw material: hawthorn 100-1500, Rhizoma Acori Calami 80-1300, shepherd's purse 50-1100, fevervine 50-1100, capsule of weeping forsythia 90-1500, loguat leaf 50-800, cicada slough 10-250, the membrane of a chicken's gizzard 50-800.Can the gastritis of treatment due to weakness of the spleen and the stomach, the indigestion that causes, halitosis abdominal distension, become thin unablely, have no peace of mind, insomnia and dreamful sleep, illness such as forgetful, children's hyperkinetic syndrome) (doctor trained in Western medicine claims: disease such as can to treat infantile malnutrition again.This disclosure of the Invention the composition of above pharmaceutical preparation, preparation method and pharmacodynamics data, but how its content is accurately measured, better its quality being controlled is problem demanding prompt solution.
In the existing national drug standards (trying) of haw and corium stomachium galli preparation,, adopted neutral alumina column chromatography purification test sample with liquid chromatography for measuring forsythin content, but more because of impurity, there is the problem that baseline is higher, degree of separation is bad.In the forsythin liquid phase chromatography assay, Chinese Pharmacopoeia most neutral alumina column chromatography purification test samples that adopt of the national drug standards such as version in 2005, SUNJU GANMAO PIAN then adopts chloroform extraction; Also useful silica gel chromatographic column, macroporous resin column purifying in the documents and materials.
Measure among the preparation method of need testing solution under the item about medicinal material or formulation content in the national drug standards, do not retrieve the method for in same chromatographic column, loading two kinds of certain compositions of filling agent purifying.
Summary of the invention
The content assaying method that the purpose of this invention is to provide a kind of haw and corium stomachium galli preparation.
The content assaying method of haw and corium stomachium galli preparation of the present invention is made up of following steps:
One, chromatographic condition and system suitability test chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica; The acetonitrile-water gradient elution, or be moving phase with acetonitrile-water (25: 75), detecting wavelength is 277nm or 230nm, number of theoretical plate calculates by the forsythin peak should be not less than 3000;
Two, it is an amount of that the preparation precision of reference substance solution takes by weighing the forsythin reference substance, adds methyl alcohol and make the solution that every 1ml contains 15 μ g, promptly;
Three, golden oral liquid in the hawthorn is got in the preparation of extract, mixing, and precision is measured 5～50ml, 2～3 times of volumes methanol of accurate adding, close plug shakes up, and places 10～30 minutes, filters, precision is measured subsequent filtrate 10～50ml, is concentrated into 25% ± 10% volume in the water-bath, as concentrate;
Or get gold size capsule content in the hawthorn, and grind well, get 1～5g, the accurate title, decide, and puts in the tool plug conical flask, adds 10～40 times of volumes methanol, close plug claims to decide weight, sonicated 30 minutes, be chilled to room temperature, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 5～50ml, the water that adds the volume of measuring 25% is concentrated into 25% ± 10% volume, as concentrate in the water-bath;
Four, the concentrate water of the purification step of need testing solution (three) moves on macroreticular resin-neutral alumina post, vessel repeatedly wash with low amounts of water, cleansing solution all moves on the post, column internal diameter 1～5cm, the bottom is 50～400 order neutral aluminas, 3～10g, top is the good macroreticular resin of pre-service of height 3～15cm, flow velocity with per minute 1～5ml passes through chromatographic column, water 50～150ml successively, 50～95% ethanolic solutions, 60～200ml wash-out is used in 10～25% ethanolic solutions, 60～200ml washing again, collects eluent, evaporate to dryness, residue adds methyl alcohol or 50% methyl alcohol makes dissolving, is transferred in 5～25ml measuring bottle, adds methyl alcohol or 50% methyl alcohol is diluted to scale, shake up, filter, get subsequent filtrate, as need testing solution;
Five, accurate respectively reference substance solution and need testing solution each 10 μ l or the 20 μ l of drawing of determination method inject liquid chromatograph, measure, promptly.
Content assaying method of the present invention is to have obtained on a large amount of experiment basis having carried out.Extracting on the choice of Solvent, the majority state drug standards adopt methyl alcohol for extracting solvent, measure the content of forsythin in medicinal material or the preparation, according to this product reality, the applicant has carried out the test of extraction solvent screening, reduce the impurity stripping quantity when attempting to guarantee extraction ratio, the result shows, several extraction ratios of solvent, methanol extraction is the most abundant, and extract impurity is few, therefore selects methyl alcohol as extracting solvent.On extracting mode, the national tentative standard of golden oral liquid adopts the evaporate to dryness oral liquid in the hawthorn, add the methyl alcohol ultrasonic Extraction, oral liquid evaporate to dryness process is very time-consuming, and if temperature is too high easily to damage tested composition, the applicant adopts oral liquid directly to add the methyl alcohol mixing, leaves standstill 10～30min, precipitation is removed most of honey, filters; This method of evidence is feasible, and it is few, simple to operate to extract impurity.On the mode of concentrating, because forsythin only can be adsorbed on the macroreticular resin in the alcoholic solution of water or low concentration, separate with other impurity, therefore, boil off methyl alcohol in the extract water-bath, stay the direct upper prop of aqueous solution, with the water solution transfer comparison again of first evaporate to dryness, operate easylier, the more important thing is easy transfer and shift fully.More unique is purification process, all there are different separately problems in existing each extract purification process such as neutral alumina, macroreticular resin, silica gel, RP-C18 column chromatography or extraction etc. through experiment, the result all is difficult to arrive the relevant technologies requirement, therefore, the applicant consider by in same post with two kinds of disposable purifying that carry out of filling agent, trial test after deliberation,, in same chromatographic column, bottom filling neutral alumina, top filling macroreticular resin, in theory relatively rationally, actual effect is also relatively good, the chromatogram effect has clear improvement, and saves time, and is easy and simple to handle.In washing process, in view of forsythin is adsorbed in the character of macroreticular resin, for the macroreticular resin on chromatographic column top, the alcoholic solution of water and low concentration (less than 30% ethanol) washing, can only fully remove those and not be adsorbed or adsorb more weak impurity, reach the purpose of purifying extract; Neutral alumina for the chromatographic column bottom, the eluting power of solvent is: (determining alcohol is low more in the alcoholic solution for water＞alcoholic solution＞alcohol, eluting power is strong more), therefore, the impurity that washs from macroreticular resin is not nearly all adsorbed by neutral alumina, the impurity of minute quantity absorption can not be eluted by eluent (50～95% ethanol) subsequently, thereby can interference measurement; In elution process, for the macroreticular resin on chromatographic column top, forsythin can be eluted fully, and the stronger impurity of a small amount of absorption is still stayed on the resin with 50～95% ethanolic solutions; Neutral alumina for the chromatographic column bottom, forsythin in 50～95% ethanolic solutions can not be adsorbed fully, thereby the recovery is higher, and follow forsythin most adsorbed from the impurity that macroreticular resin elutes by neutral alumina by 50～95% ethanolic solutions, further reach the purpose of purifying extract.Through comprehensive evaluation, in conjunction with each system suitability parameter situation, and through the methodology checking, indexs such as this method accuracy (average recovery), repeatability, specificity are all relatively good, reach national drug standards requirement.
Embodiment
Embodiment 1: the assay of golden oral liquid in the hawthorn
Get hawthorn 218g, Rhizoma Acori Calami 141g, shepherd's purse 115g, fevervine 115g, capsule of weeping forsythia 192g, loguat leaf 90g, cicada slough 39g, the membrane of a chicken's gizzard 90g.Soak, decoct secondary, 1.5 hours for the first time, 1 hour for the second time, collecting decoction filtered, filtrate is concentrated into the clear cream that relative density is 1.03～1.06 (55～65 ℃), add honey, honey element, potassium sorbate, add water to ormal weight, stir evenly, filter, can, oral liquid 1000ml is made in sterilization.
This product 30ml is got in [discriminating] (1), extracts 3 times with water saturated normal butyl alcohol jolting, each 15ml, merge normal butyl alcohol liquid,, divide and get normal butyl alcohol liquid with the saturated water 30ml washing of normal butyl alcohol, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, and solution is by neutral alumina post (120 orders, 3g, internal diameter 10mm, wet method dress post, use methyl alcohol prewashing), with methyl alcohol 80ml wash-out, collect eluent, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.Other gets fevervine control medicinal material 3.5g, adds water 100ml, and little boiling decocted 30 minutes, filtered, and filtrate is concentrated into 30ml, handles with method, and residue adds methyl alcohol 0.5ml makes dissolving, in contrast medicinal material solution.Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), drawing each 5 μ l of above-mentioned two kinds of solution puts respectively on same silica gel g thin-layer plate, with methenyl choloride-methyl alcohol-strong aqua (9: 2: 0.2) is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, put under 105 ℃ and dry by the fire, inspect under the daylight to clear spot.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
(2) get this product 30ml, extract 3 times with water saturated normal butyl alcohol jolting, each 15ml merges normal butyl alcohol liquid, with the saturated water 30ml washing of normal butyl alcohol, divides and gets normal butyl alcohol liquid, and evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.Other gets loguat leaf control medicinal material 3g, adds water 100ml, and little boiling decocted 30 minutes, filtered, and filtrate is concentrated into 30ml, handles with method, and residue adds methyl alcohol 1ml makes dissolving, in contrast medicinal material solution.Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-glacial acetic acid (16: 8: 0.1) is developping agent, launches, and takes out, dry, spray is put under 105 ℃ and is dried by the fire to clear spot with 10% ethanol solution of sulfuric acid, inspects under the daylight.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
(3) in the chromatogram that [assay] writes down down, should present in the test sample chromatogram with the reference substance chromatogram in the identical chromatographic peak of main peak retention time.
[inspection] relative density should be not less than 1.03 (appendix VIIA of Chinese Pharmacopoeia version in 2005).
The pH value should be 4.0～6.0 (appendix VIIG of Chinese Pharmacopoeia version in 2005).
Other should meet every regulation relevant under the mixture item (appendix IJ of Chinese Pharmacopoeia version in 2005).
[assay] measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test are filling agent with the octadecylsilane chemically bonded silica; With the acetonitrile is mobile phase A, is Mobile phase B with water, and the regulation in the according to the form below is carried out gradient elution; The detection wavelength is 230nm.Number of theoretical plate calculates by the forsythin peak should be not less than 3000.
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0～15 15～20 20～30 | 22 22～25 25～28 | 78 78～75 75～72 |
It is an amount of that the forsythin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds 50% methyl alcohol and makes the solution that every 1ml contains 15 μ g, promptly.
This product under the loading amount item is got in the preparation of need testing solution, mixing, precision is measured 10ml, the accurate methyl alcohol 25ml that adds, close plug, mixing was placed 10 minutes, filtered, precision is measured subsequent filtrate 20ml, be concentrated into about 5ml in the water-bath, water shifts and slowly adds to macroreticular resin-neutral alumina post (internal diameter 2cm, wet method dress post; The bottom is 100～200 order neutral alumina 5g; Top is the good D101 macroreticular resin of pre-service of height 6cm) on, leave standstill 10 minutes after, pass through chromatographic column with the flow velocity of per minute 2～3ml, 50% ethanolic solution 80ml wash-out is used in water 50ml, 20% ethanolic solution 80ml washing successively again, collects eluent, evaporate to dryness, residue adds 50% methyl alcohol makes dissolving, is transferred in the 5ml measuring bottle, adds 50% methyl alcohol and is diluted to scale, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly.
Every of this product contains the capsule of weeping forsythia with forsythin (C
27H
34O
11) meter, must not be less than 100 μ g.
Embodiment 2: the assay of gold size capsule in the hawthorn
Get hawthorn 1090g, Rhizoma Acori Calami 705g, shepherd's purse 575g, fevervine 575g, capsule of weeping forsythia 960g, loguat leaf 450g, cicada slough 195g, the membrane of a chicken's gizzard 450g, soak 12 hours after, decoct secondary, 1.5 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate is concentrated into the thick paste that relative density is 1.20～1.22 (60 ℃), drying, be ground into powder, add starch, mixing, make particle, drying adds talcum powder, dolomol, mixing incapsulates, and makes 1000 of capsules.
This product content 2g is got in [discriminating] (1), adds water 30ml, puts in 60 ℃ of water-baths temperature and soaks 30 minutes, centrifugal, get supernatant and be transferred in the separating funnel, extract 3 times with water saturated normal butyl alcohol jolting, each 15ml, merge normal butyl alcohol liquid,, divide and get normal butyl alcohol liquid with the saturated water 30ml washing of normal butyl alcohol, evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, and solution is by neutral alumina post (120 orders, 3g, internal diameter 10mm, wet method dress post is used methyl alcohol prewashing), with methyl alcohol 80ml wash-out, collect eluent, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.Other gets fevervine control medicinal material 3.5g, adds water 100ml, and little boiling decocted 30 minutes, filtered, and filtrate is concentrated into 30ml, handles with method, and residue adds methyl alcohol 0.5ml makes dissolving, in contrast medicinal material solution.Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with methenyl choloride-methyl alcohol-strong aqua (9: 2: 0.2) is developping agent, launches, and takes out, dry, spray is put under 105 ℃ and is dried by the fire to clear spot with 10% ethanol solution of sulfuric acid, inspects under the daylight.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
(2) get this product content 2g, add water 30ml, put in 60 ℃ of water-baths temperature and soaked 30 minutes, be transferred in the separating funnel, extract 3 times with water saturated normal butyl alcohol jolting, each 15ml merges normal butyl alcohol liquid, with the saturated water 30ml washing of normal butyl alcohol, divide and get normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 1ml makes dissolving, as need testing solution.Other gets loguat leaf control medicinal material 3g, adds water 100ml, and little boiling decocted 30 minutes, filtered, and filtrate is concentrated into 30ml, handles with method, and residue adds methyl alcohol 1ml makes dissolving, in contrast medicinal material solution.Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane-ethyl acetate-glacial acetic acid (16: 8: 0.1) is developping agent, launches, and takes out, dry, spray is put under 105 ℃ and is dried by the fire to clear spot with 10% ethanol solution of sulfuric acid, inspects under the daylight.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
(3) in the chromatogram that [assay] writes down down, should present in the test sample chromatogram with the reference substance chromatogram in the identical chromatographic peak of main peak retention time.
[inspection] should meet every regulation relevant under the capsule item (appendix IL of Chinese Pharmacopoeia version in 2005).
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filling agent with the octadecylsilane chemically bonded silica; With the acetonitrile is mobile phase A, is Mobile phase B with water, and the regulation in the according to the form below is carried out gradient elution; The detection wavelength is 230nm.Number of theoretical plate calculates by the forsythin peak should be not less than 3000.
| Time (minute) | Mobile phase A (%) | Mobile phase B (%) |
| 0～15 15～20 20～30 | 22 22～25 25～28 | 78 78～75 75～72 |
It is an amount of that the forsythin reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds 50% methyl alcohol and makes the solution that every 1ml contains 15 μ g, promptly.
The content under this product content uniformity item is got in the preparation of need testing solution, grinds well, and gets 1g, and accurate the title decides, put in the tool plug conical flask accurate methyl alcohol 25ml, the close plug of adding, claim to decide weight, sonicated 30 minutes is chilled to room temperature, claim again to decide weight, supply the weight that subtracts mistake, shake up with methyl alcohol, filter, precision is measured subsequent filtrate 10ml, adds water 5ml, be concentrated into about 5ml in the water-bath, water is transferred to macroreticular resin-neutral alumina post (internal diameter 2cm, wet method dress post; The bottom is 100～200 order neutral alumina 5g; Top is the good D101 macroreticular resin of pre-service of height 6cm) on, with the flow velocity of per minute 2～3ml by chromatographic column, water 50ml, 20% ethanolic solution 80ml washing successively, use 50% ethanolic solution 80ml wash-out again, collect eluent, evaporate to dryness, residue add 50% methyl alcohol makes dissolving, be transferred in the 5ml measuring bottle, add 50% methyl alcohol and be diluted to scale, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly.
Every of this product contains the capsule of weeping forsythia with forsythin (C
27H
34O
11) meter, must not be less than 70 μ g.
Claims (1)
1. the content assaying method of a haw and corium stomachium galli preparation, described haw and corium stomachium galli preparation is the medicament of being made by the following weight proportion raw material: hawthorn 100-1500, Rhizoma Acori Calami 80-1300, shepherd's purse 50-1100, fevervine 50-1100, capsule of weeping forsythia 90-1500, loguat leaf 50-800, cicada slough 10-250, the membrane of a chicken's gizzard 50-800; Its content assaying method is made up of following steps:
One, the test of chromatographic condition and system suitability is a filling agent with octadecylsilane chemically bonded silica; The acetonitrile-water gradient elution, or be moving phase with 25: 75 acetonitrile-water, detecting wavelength is 277nm or 230nm, number of theoretical plate calculates by the forsythin peak should be not less than 3000;
Two, it is an amount of that the preparation precision of reference substance solution takes by weighing the forsythin reference substance, adds methyl alcohol and make the solution that every 1ml contains 15 μ g, promptly;
Three, the preparation of extract
Four, the concentrate of the purification step of extract (three) moves on macroreticular resin-neutral alumina post, vessel repeatedly wash with low amounts of water, cleansing solution all moves on the post, flow velocity with per minute 1～5ml passes through chromatographic column, water 50～150ml successively, 10～25% ethanolic solutions, 60～200ml washing, use 50～95% ethanolic solutions, 60～200ml wash-out again, collect eluent, evaporate to dryness, residue add methyl alcohol or 50% methyl alcohol makes dissolving, be transferred in 5～25ml measuring bottle, add methyl alcohol or 50% methyl alcohol is diluted to scale, shake up, filter, get subsequent filtrate, as need testing solution;
Five, accurate respectively reference substance solution and need testing solution each 10 μ l or the 20 μ l of drawing of determination method inject liquid chromatograph, measure, promptly;
It is characterized in that:
The preparation process of step (three) extract is: get golden oral liquid in the hawthorn, mixing, precision is measured 5～50ml, accurate 2～3 times of volumes methanol, the close plug of adding, shake up, placed 10～30 minutes, and filtered, precision is measured subsequent filtrate 10～50ml, be concentrated into 25% ± 10% volume in the water-bath, as concentrate;
Or get gold size capsule content in the hawthorn, and grind well, get 1～5g, the accurate title, decide, and puts in the tool plug conical flask, adds 10～40 times of volumes methanol, close plug claims to decide weight, sonicated 30 minutes, be chilled to room temperature, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, precision is measured subsequent filtrate 5～50ml, the water that adds the volume of measuring 25% is concentrated into 25% ± 10% volume, as concentrate in the water-bath; Macroreticular resin-the neutral alumina column internal diameter is 1～5cm in the above-mentioned steps (four), and the bottom is 50～400 order neutral aluminas, 3～10g, and top is the good macroreticular resin of pre-service of height 3～15cm.
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| 王慧琛.HPLC法测定桑姜感冒片中连翘苷.中草药37 5.2006,37(5),713-714. |
| 王慧琛.HPLC法测定桑姜感冒片中连翘苷.中草药37 5.2006,37(5),713-714. * |
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