CN103175910A - Method for controlling quality of liquorice and liquorice preparation - Google Patents
Method for controlling quality of liquorice and liquorice preparation Download PDFInfo
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- CN103175910A CN103175910A CN2013100378218A CN201310037821A CN103175910A CN 103175910 A CN103175910 A CN 103175910A CN 2013100378218 A CN2013100378218 A CN 2013100378218A CN 201310037821 A CN201310037821 A CN 201310037821A CN 103175910 A CN103175910 A CN 103175910A
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- isoliquiritin
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- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 23
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 title claims abstract description 13
- 244000303040 Glycyrrhiza glabra Species 0.000 title abstract description 11
- 235000011477 liquorice Nutrition 0.000 title abstract 10
- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229960004949 glycyrrhizic acid Drugs 0.000 claims abstract description 27
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 claims abstract description 27
- 235000019410 glycyrrhizin Nutrition 0.000 claims abstract description 27
- 238000012360 testing method Methods 0.000 claims abstract description 21
- MPDGHEJMBKOTSU-YKLVYJNSSA-N 18beta-glycyrrhetic acid Chemical compound C([C@H]1C2=CC(=O)[C@H]34)[C@@](C)(C(O)=O)CC[C@]1(C)CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@H](O)C1(C)C MPDGHEJMBKOTSU-YKLVYJNSSA-N 0.000 claims abstract description 14
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001685 glycyrrhizic acid Substances 0.000 claims abstract description 14
- JBQATDIMBVLPRB-UHFFFAOYSA-N isoliquiritigenin Natural products OC1=CC(O)=CC=C1C1OC2=CC(O)=CC=C2C(=O)C1 JBQATDIMBVLPRB-UHFFFAOYSA-N 0.000 claims abstract description 14
- GSZUGBAEBARHAW-UHFFFAOYSA-N sophoraflavone B Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C=2OC3=CC(O)=CC=C3C(=O)C=2)C=C1 GSZUGBAEBARHAW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003908 quality control method Methods 0.000 claims abstract description 13
- KSDSYIXRWHRPMN-UHFFFAOYSA-N 4'-O-beta-D-Galactopyranoside-6''-p-Coumaroylprunin-4',5,7-Trihydroxyflavanone Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C2OC3=CC(O)=CC(O)=C3C(=O)C2)C=C1 KSDSYIXRWHRPMN-UHFFFAOYSA-N 0.000 claims abstract description 12
- MPDGHEJMBKOTSU-UHFFFAOYSA-N Glycyrrhetinsaeure Natural products C12C(=O)C=C3C4CC(C)(C(O)=O)CCC4(C)CCC3(C)C1(C)CCC1C2(C)CCC(O)C1(C)C MPDGHEJMBKOTSU-UHFFFAOYSA-N 0.000 claims abstract description 12
- YNWXJFQOCHMPCK-UHFFFAOYSA-N Isoliquiritin Natural products OC1C(O)C(O)C(CO)OC1OC(C=C1)=CC=C1C=CC(=O)C1=CC=C(O)C=C1O YNWXJFQOCHMPCK-UHFFFAOYSA-N 0.000 claims abstract description 12
- DEMKZLAVQYISIA-ONJCETCRSA-N Liquiritin Natural products O([C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1)c1ccc([C@@H]2Oc3c(C(=O)C2)ccc(O)c3)cc1 DEMKZLAVQYISIA-ONJCETCRSA-N 0.000 claims abstract description 12
- DEMKZLAVQYISIA-UHFFFAOYSA-N Liquirtin Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C2OC3=CC(O)=CC=C3C(=O)C2)C=C1 DEMKZLAVQYISIA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229960003720 enoxolone Drugs 0.000 claims abstract description 12
- DXDRHHKMWQZJHT-FPYGCLRLSA-N isoliquiritigenin Chemical compound C1=CC(O)=CC=C1\C=C\C(=O)C1=CC=C(O)C=C1O DXDRHHKMWQZJHT-FPYGCLRLSA-N 0.000 claims abstract description 12
- 235000008718 isoliquiritigenin Nutrition 0.000 claims abstract description 12
- YNWXJFQOCHMPCK-LXGDFETPSA-N isoliquiritin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC(C=C1)=CC=C1\C=C\C(=O)C1=CC=C(O)C=C1O YNWXJFQOCHMPCK-LXGDFETPSA-N 0.000 claims abstract description 12
- DEMKZLAVQYISIA-ZRWXNEIDSA-N liquiritin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C([C@H]2OC3=CC(O)=CC=C3C(=O)C2)C=C1 DEMKZLAVQYISIA-ZRWXNEIDSA-N 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 24
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 18
- 239000004378 Glycyrrhizin Substances 0.000 claims description 13
- 239000013558 reference substance Substances 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 241000202807 Glycyrrhiza Species 0.000 claims description 11
- WNIFXKPDILJURQ-UHFFFAOYSA-N stearyl glycyrrhizinate Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CCC5(C)CCC(C(=O)OCCCCCCCCCCCCCCCCCC)(C)CC5C4=CC(=O)C3C21C WNIFXKPDILJURQ-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- LTINPJMVDKPJJI-UHFFFAOYSA-N iodinated glycerol Chemical compound CC(I)C1OCC(CO)O1 LTINPJMVDKPJJI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000004811 liquid chromatography Methods 0.000 claims description 4
- 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
- 235000001453 Glycyrrhiza echinata Nutrition 0.000 claims description 3
- 235000017382 Glycyrrhiza lepidota Nutrition 0.000 claims description 3
- 238000004587 chromatography analysis Methods 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 229940010454 licorice Drugs 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 238000002137 ultrasound extraction Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 6
- 238000004128 high performance liquid chromatography Methods 0.000 abstract description 4
- 238000011835 investigation Methods 0.000 abstract description 2
- FURUXTVZLHCCNA-UHFFFAOYSA-N Liquiritigenin Natural products C1=CC(O)=CC=C1C1OC2=CC(O)=CC=C2C(=O)C1 FURUXTVZLHCCNA-UHFFFAOYSA-N 0.000 abstract 2
- 239000004480 active ingredient Substances 0.000 abstract 2
- FURUXTVZLHCCNA-AWEZNQCLSA-N liquiritigenin Chemical compound C1=CC(O)=CC=C1[C@H]1OC2=CC(O)=CC=C2C(=O)C1 FURUXTVZLHCCNA-AWEZNQCLSA-N 0.000 abstract 2
- 230000007547 defect Effects 0.000 abstract 1
- 238000003556 assay Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000005464 sample preparation method Methods 0.000 description 2
- DLHXRDUXNVEIEY-UHFFFAOYSA-N 7-Methylcoumarin Chemical compound C1=CC(=O)OC2=CC(C)=CC=C21 DLHXRDUXNVEIEY-UHFFFAOYSA-N 0.000 description 1
- CJIJXIFQYOPWTF-UHFFFAOYSA-N 7-hydroxycoumarin Natural products O1C(=O)C=CC2=CC(O)=CC=C21 CJIJXIFQYOPWTF-UHFFFAOYSA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- PVKQULHHWVQXLE-UHFFFAOYSA-N Glycyrol Natural products C12=CC=C(O)C=C2OC2=C1C(=O)OC1=C2C(O)=C(CC=C(C)C)C(OC)=C1 PVKQULHHWVQXLE-UHFFFAOYSA-N 0.000 description 1
- 241001278898 Glycyrrhiza inflata Species 0.000 description 1
- 240000008917 Glycyrrhiza uralensis Species 0.000 description 1
- 235000000554 Glycyrrhiza uralensis Nutrition 0.000 description 1
- GFJNBLOMWYSKSS-UHFFFAOYSA-N Isoglycyrol Natural products COc1c2CCC(C)(C)Oc2cc3OC(=O)c4c(oc5c(O)cccc45)c13 GFJNBLOMWYSKSS-UHFFFAOYSA-N 0.000 description 1
- XQWFHGOIUZFQPJ-USTPAGJBSA-N Neoisoliquiritigenin Natural products O=C(/C=C/c1ccc(O)cc1)c1c(O)cc(O[C@H]2[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O2)cc1 XQWFHGOIUZFQPJ-USTPAGJBSA-N 0.000 description 1
- XQWFHGOIUZFQPJ-LXGDFETPSA-N Neoisoliquiritin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC(C=C1O)=CC=C1C(=O)\C=C\C1=CC=C(O)C=C1 XQWFHGOIUZFQPJ-LXGDFETPSA-N 0.000 description 1
- XQWFHGOIUZFQPJ-UHFFFAOYSA-N Neoisoliquiritin Natural products OC1C(O)C(O)C(CO)OC1OC(C=C1O)=CC=C1C(=O)C=CC1=CC=C(O)C=C1 XQWFHGOIUZFQPJ-UHFFFAOYSA-N 0.000 description 1
- HJBUYKZTEBZNSH-ZRWXNEIDSA-N Neoliquiritin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C(C(=O)C[C@H](O2)C=3C=CC(O)=CC=3)C2=C1 HJBUYKZTEBZNSH-ZRWXNEIDSA-N 0.000 description 1
- HJBUYKZTEBZNSH-ONJCETCRSA-N Neoliquiritin Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C(C(=O)C[C@@H](O2)C=3C=CC(O)=CC=3)C2=C1 HJBUYKZTEBZNSH-ONJCETCRSA-N 0.000 description 1
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N benzo-alpha-pyrone Natural products C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
- 150000004775 coumarins Chemical class 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- LWESBHWAOZORCQ-UHFFFAOYSA-N glycyrol Chemical compound C12=CC=C(O)C=C2OC2=C1C(=O)OC1=C2C(OC)=C(CC=C(C)C)C(O)=C1 LWESBHWAOZORCQ-UHFFFAOYSA-N 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 238000010262 high-speed countercurrent chromatography Methods 0.000 description 1
- CFWLRXJPRRCJTI-UHFFFAOYSA-N iso-glycyrol Chemical compound C12=CC=C(O)C=C2OC2=C1C(=O)OC1=C2C(OC)=C(CCC(C)(C)O2)C2=C1 CFWLRXJPRRCJTI-UHFFFAOYSA-N 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003648 triterpenes Chemical class 0.000 description 1
- ORHBXUUXSCNDEV-UHFFFAOYSA-N umbelliferone Chemical compound C1=CC(=O)OC2=CC(O)=CC=C21 ORHBXUUXSCNDEV-UHFFFAOYSA-N 0.000 description 1
- HFTAFOQKODTIJY-UHFFFAOYSA-N umbelliferone Natural products Cc1cc2C=CC(=O)Oc2cc1OCC=CC(C)(C)O HFTAFOQKODTIJY-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a method for controlling quality of a liquorice medicinal material and a liquorice preparation. The method concretely relates to the step of simultaneously determining the content of the liquorice medicinal material and the content of six main active ingredients, namely liquiritin, isoliquiritin, liquiritigenin, isoliquiritigenin, glycyrrhizic acid and glycyrrhetinic acid in the liquorice preparation by utilizing a high performance liquid chromatography. A new method for controlling the quality of the liquorice and the liquorice preparation is established and the six main active ingredients, namely liquiritin, isoliquiritin, liquiritigenin, isoliquiritigenin, glycyrrhizic acid and glycyrrhetinic acid are quantitatively determined simultaneously by utilizing the high performance liquid chromatography. Confirmed by methodological investigation and test, the method is simple and convenient, correct in result and good in reproducibility, the defect of the existing quality control is overcome, and the quality control on the liquorice and the liquorice preparation is perfect and scientific.
Description
Technical field:
The present invention relates to the method for quality control of licorice medicinal materials and preparation thereof, be specifically related to: the content of the liquiritin in this medicinal material of hplc simultaneous determination and preparation thereof, isoliquiritin, glycyrrhizin, isoliquiritigenin, glycyrrhizic acid, six kinds of main active of enoxolone.
Background technology:
Radix Glycyrrhizae is the dry root and rhizome of pulse family glycyrrhiza genus Radix Glycyrrhizae Glycyrrhiza uralensis Fisch, glycyrrhiza inflate bat Glycyrrhiza inflata Bat or glycyrrhiza glabra Glycyrrhiza glabra L, is one of the most frequently used Important Chinese Medicinal Herbs material.Before two thousand years, Shennong's Herbal is just classified Radix Glycyrrhizae on medicine as and is taken advantage of.China's traditional Chinese medical science thinks, Radix Glycyrrhizae is invigorated the spleen and benefited qi, and grows to cough moistening lung, and the emergency detoxifcation is in harmonious proportion hundred medicines, therefore saying of " ten side's nine grass " is arranged, and enjoys the good reputation of " king of Chinese herbal medicine ".
The chemical composition of Radix Glycyrrhizae is very complicated, scholar both domestic and external is studied it in different fields, so far from Radix Glycyrrhizae isolated compound more than the 100 kind of compounds such as Coumarins, triterpenes and flavonoids such as glycyrrhizin, enoxolone, liquiritin, isoliquiritin, Neoliquiritin, Neoisoliquiritin, glycyrrhizin, isoliquiritigenin and glycyrol, isoglycyrol, 7-methylcoumarin essence, umbelliferone are arranged, all have physiologically active widely.
At present Radix Glycyrrhizae and preparation thereof are carried out the research of quality control a lot, also set up a lot of quantitative analysis methods simultaneously, as gas phase-mass spectrometry, liquid phase-mass spectrometry, high-speed countercurrent chromatography etc.But these methods are just carried out quality control to a or two composition in Radix Glycyrrhizae, can't embody licorice medicinal materials and contain the full-quality of Radix Glycyrrhizae Chinese patent medicine preparation, and very high to the instrument of instrument, find in the practice examining operation simultaneously, said method exists that specificity is poor, complex operation, poor controllability, the assay deficiency such as poor stability as a result, but affects the generalization of standard.
Summary of the invention
The objective of the invention is to formulate new Radix Glycyrrhizae and the method for quality control of preparation thereof, utilize hplc simultaneous determination liquiritin, isoliquiritin, glycyrrhizin, isoliquiritigenin, glycyrrhizic acid, six kinds of main active of enoxolone to carry out quantitative measurement, investigate test through methodology, confirm that the method is easy, result is accurate, favorable reproducibility, made up the deficiency of existing quality control, the quality control of Radix Glycyrrhizae and preparation thereof is improved and science more.
The assay method of Radix Glycyrrhizae of the present invention and the quality control of preparation high performance liquid chromatography thereof comprises the steps:
The method of quality control of a kind of Radix Glycyrrhizae and preparation thereof is:
(1) efficient liquid phase chromatographic analysis: chromatographic condition chromatographic column: Agilent HC-C
18Post (4.6mm * 250mm, 5 μ m); Mobile phase: acetonitrile: 0.04% formic acid solution; Adopt the gradient elution mode: 0min → 4min → 20min → 25min → 38min → 50min → 60min, acetonitrile 20% → 20% → 38% → 55% → 90% → 90% → 20%; Flow velocity: 1mlmin
-1Column temperature: 30 ℃; Detect wavelength: 250nm, 365nm, number of theoretical plate should be not less than 2000 by glycyrrhizic acid;
(2) preparation of need testing solution: the test sample of Radix Glycyrrhizae or glycyrrhiza preparation is ground into the 20-40 order, precision takes Radix Glycyrrhizae powder 0.15g or glycyrrhiza preparation powder 0.25g, precision adds 8ml50% alcohol immersion 30min, then ultrasonic extraction 30min, filter after being placed to room temperature, filtrate is settled to 10ml with 50% ethanol, filters with miillpore filter (0.45 μ m), get subsequent filtrate, as need testing solution;
(3) preparation of reference substance solution: precision takes liquiritin, glycyrrhizin, glycyrrhizic acid, isoliquiritin, isoliquiritigenin, six kinds of reference substances of enoxolone respectively, adds methyl alcohol and dissolves and be made into liquiritin 1.728 mgml
-1, glycyrrhizin 2.736 mgml
-1, glycyrrhizic acid 4.680 mgml
-1, isoliquiritin 2.016 mgml
-1, isoliquiritigenin 0.612 mgml
-1, enoxolone 0.540 mgml
-1Storing solution;
(4) content assaying method: precision is drawn reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, the content of six kinds of compositions of mensuration respectively.
It is testing index that the present invention has selected six kinds of active components in Radix Glycyrrhizae and preparation thereof, and carries out following methods and learn the investigation test:
1. accurate reference substance solution 0.2ml, 0.4ml, 0.6ml, 0.8ml, the 1.0ml of drawing of the range of linearity, add methanol constant volume to 1ml.By above-mentioned chromatographic condition 10 μ l sample introductions, take the peak area x that records as horizontal ordinate, sample quality y is ordinate, calculates regression equation.Result shows, reference substance peak area and concentration are good linear relationship.The results are shown in Table 1.
Regression equation and the range of linearity of six kinds of main active of table 1
2. precision is got reference substance solution, measures by the method under the drafting item of typical curve, and RSD is respectively 0.917%, 1.128%, 1.052%, 3.884%, 1.945%, 3.487% as a result, shows that method precision is good.
3. stability is got need testing solution, presses the method under the drafting item of typical curve, is measuring at 0,4,8,12,24h respectively.RSD is respectively 2.069%, 2.129%, 1.484%, 3.197%, 2.565%, 3.457% as a result, shows that sample is good at 24 hours internal stabilities.
4. reappearance is got with a collection of test sample appropriate (n=5), accurately weighed respectively, after processing according to above-mentioned test sample preparation method, carry out assay, RSD is respectively 1.389%, 3.015%, 2.551%, 1.494%, 2.540%, 1.882% as a result, and result shows that the method reappearance is good.
5. the accurate sample that takes known content of average recovery test is 3 parts, and precision adds reference substance appropriate respectively, after processing according to above-mentioned test sample preparation method, carries out assay, and experimental result sees Table 2.
Table 2 average recovery result
By above-mentioned 5 tests as can be known, the assay method of Radix Glycyrrhizae of the present invention and the quality control of preparation high performance liquid chromatography thereof has advantages of that linear relationship is good, precision is high, good stability, favorable reproducibility, average recovery be high.
Description of drawings
Fig. 1 represents in a reason six kinds of main active assay liquid chromatograms in ball;
Fig. 2 represents six kinds of main active assay liquid chromatograms in b compound glycyrrhizin sheet;
Fig. 3 represents six kinds of main active assay liquid chromatograms in the c Liu Yi San;
Fig. 4 represents six kinds of main active assay liquid chromatograms in the d Brown Mixtura.
Embodiment
The present invention will be described in detail below in conjunction with embodiment, and embodiment does not consist of any restriction of the present invention.
Embodiment:
Content with liquiritin, isoliquiritin, glycyrrhizin, isoliquiritigenin, glycyrrhizic acid, six kinds of main active of enoxolone in ball, b compound glycyrrhizin sheet, c Liu Yi San, four kinds of glycyrrhiza preparations of d Brown Mixtura in high effective liquid chromatography for measuring a reason.
The instrument that uses has: high performance liquid chromatograph (Agilent 1100 series: Agilent G1311A pump, Agilent G1316A UV-detector, Agilent G1313A automatic sampler); SL4001N electronic balance (the accurate scientific and technological Instr Ltd. of Shanghai Min Qiao); Ultrasonic oscillator (power 300W, frequency 40kHz).
(1) efficient liquid phase chromatographic analysis chromatographic condition chromatographic column: Agilent HC-C
18Post (4.6mm * 250mm, 5 μ m); Mobile phase: acetonitrile: 0.04% formic acid solution; Adopt the gradient elution mode: 0min → 4min → 20min → 25min → 38min → 50min → 60min, acetonitrile 20% → 20% → 38% → 55% → 90% → 90% → 20%; Flow velocity: 1mlmin
-1Column temperature: 30 ℃; Detect wavelength: 250nm, 365nm, number of theoretical plate should be not less than 2000 by glycyrrhizic acid.
(2) preparation of reference substance solution: accurately respectively take six kinds of reference substances in right amount in the volumetric flask of 10ml, add methyl alcohol and dissolve and be made into liquiritin 1.728 mgml
-1, glycyrrhizin 2.736 mgml
-1, glycyrrhizic acid 4.680 mgml
-1, isoliquiritin 2.016 mgml
-1, isoliquiritigenin 0.612 mgml
-1, enoxolone 0.540 mgml
-1Storing solution.
(3) preparation of need testing solution: four kinds of glycyrrhiza preparations are ground to form fine powder, precision takes above-mentioned each 0.25g of preparation powder, precision adds 8ml50% alcohol immersion 30min, then ultrasonic extraction 30min, filter after being placed to room temperature, filtrate is settled to 10ml with 50% ethanol, filters with miillpore filter (0.45 μ m), get subsequent filtrate, as need testing solution.
(4) content assaying method: precision is drawn reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, the content of six kinds of compositions of mensuration respectively.
Measurement result is referring to Fig. 1 ~ 4, and in each figure, the other arabic numeral 1 ~ 6 of each peak value of curve represent respectively liquiritin, isoliquiritin, glycyrrhizin, isoliquiritigenin, glycyrrhizic acid, six kinds of active components of enoxolone.
Claims (1)
1. the method for quality control of a Radix Glycyrrhizae and preparation thereof is characterized in that:
(1) efficient liquid phase chromatographic analysis: chromatographic condition chromatographic column: Agilent HC-C
18Post (4.6mm * 250mm, 5 μ m); Mobile phase: acetonitrile: 0.04% formic acid solution; Adopt the gradient elution mode: 0min → 4min → 20min → 25min → 38min → 50min → 60min, acetonitrile 20% → 20% → 38% → 55% → 90% → 90% → 20%; Flow velocity: 1mlmin
-1Column temperature: 30 ℃; Detect wavelength: 250nm, 365nm, number of theoretical plate should be not less than 2000 by glycyrrhizic acid;
(2) preparation of need testing solution: licorice powder is broken into the 20-40 order, perhaps the test sample with glycyrrhiza preparation grinds to form fine powder, precision takes Radix Glycyrrhizae powder 0.15g or glycyrrhiza preparation powder 0.25g, precision adds 8ml50% alcohol immersion 30min, and ultrasonic extraction 30min then filters after being placed to room temperature, filtrate is settled to 10ml with 50% ethanol, filter with miillpore filter (0.45 μ m), get subsequent filtrate, as need testing solution;
(3) preparation of reference substance solution: precision takes liquiritin, glycyrrhizin, glycyrrhizic acid, isoliquiritin, isoliquiritigenin, six kinds of reference substances of enoxolone respectively, adds methyl alcohol and dissolves and be made into liquiritin 1.728 mgml
-1, glycyrrhizin 2.736 mgml
-1, glycyrrhizic acid 4.680 mgml
-1, isoliquiritin 2.016 mgml
-1, isoliquiritigenin 0.612 mgml
-1, enoxolone 0.540 mgml
-1Storing solution;
(4) content assaying method: precision is drawn reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, the content of six kinds of compositions of mensuration respectively.
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| CN103940749A (en) * | 2014-03-21 | 2014-07-23 | 重庆市中药研究院 | Method for detecting storage condition of lonicera macranthoides bud medicinal material |
| CN104198599A (en) * | 2014-07-31 | 2014-12-10 | 甘肃中天药业有限责任公司 | Method for detecting glycyrrhiza uralensis |
| CN106053649A (en) * | 2016-06-12 | 2016-10-26 | 江苏天晟药业股份有限公司 | Method for detecting alpha-glycyrrhetinic acid content |
| CN109932448A (en) * | 2019-03-29 | 2019-06-25 | 完美（广东）日用品有限公司 | Content determination method for active ingredients in broom larvas and products thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103940749A (en) * | 2014-03-21 | 2014-07-23 | 重庆市中药研究院 | Method for detecting storage condition of lonicera macranthoides bud medicinal material |
| CN104198599A (en) * | 2014-07-31 | 2014-12-10 | 甘肃中天药业有限责任公司 | Method for detecting glycyrrhiza uralensis |
| CN106053649A (en) * | 2016-06-12 | 2016-10-26 | 江苏天晟药业股份有限公司 | Method for detecting alpha-glycyrrhetinic acid content |
| CN109932448A (en) * | 2019-03-29 | 2019-06-25 | 完美（广东）日用品有限公司 | Content determination method for active ingredients in broom larvas and products thereof |
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Application publication date: 20130626 |