CN105004800A - Quality detection method of cool and refreshing sunstroke prevention agent - Google Patents
Quality detection method of cool and refreshing sunstroke prevention agent Download PDFInfo
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- CN105004800A CN105004800A CN201510313272.1A CN201510313272A CN105004800A CN 105004800 A CN105004800 A CN 105004800A CN 201510313272 A CN201510313272 A CN 201510313272A CN 105004800 A CN105004800 A CN 105004800A
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Abstract
The invention discloses a quality detection method of a cool and refreshing sunstroke prevention agent. The quality detection method comprises the following steps that 1, identification is performed, namely lalang grass rhizomes are identified; 2, the content of glycyrrhizic acid is determined, namely (a) a comparison product solution is prepared, (b) a test product solution is prepared, (c) chromatographic conditions are that octadecyl silane chemically bonded silica gel serves as a filling agent, acetonitrile-water-glacial acetic acid (37:63:2.1) serves as a mobile phase, wave length is controlled to be 254 nm and the number, calculated according to the peak of the glycyrrhizic acid, of theoretical plates is not smaller than 3000, and (d) the content is determined, 10 micro-liters of comparison product solution and 10 micro-liters of test product solution are respectively and precisely sucked and then are injected into a liquid chromatograph for determination, and the content of the glycyrrhizic acid in a sample is calculated. By means of the quality detection method, the product quality of the cool and refreshing sunstroke prevention agent can be quantitatively controlled, and operation is convenient.
Description
Technical field
The invention belongs to the quality testing field of Chinese medicine preparation, relate in particular to a kind of quality determining method of refrigerant heatstroke prevention preparation.
Background technology
Refrigerant its prescription of heatstroke prevention preparation is: cogongrass rhizome 300g, lophatherum gracile 300g, eleusine indica 300g reed rhizome 300g, talcum (flying) 180g, Radix Glycyrrhizae 60g make 1000g.Its preparation technology: above Six-element, boiling secondary, 2 hours first times, second time 1 hour, collecting decoction, filter, filtrate is concentrated into cream clearly, adds cane sugar powder appropriate, makes particle, dry, is distributed into 100 bags, obtains final product.Effect: there is clearing summer heat, the effect that diuresis is promoted the production of body fluid.For hot summer weather, body heat, dry, red and prevention heatstroke of urinating, successful.Due to Chinese traditional compound medicine complicated component, both without any discriminating in former ministerial standard, more without quantitative target, therefore can not effective control for product quality.
Summary of the invention
The object of the invention is to overcome above-mentioned shortcoming and the one provided can fixing quantity product quality, the quality determining method of refrigerant heatstroke prevention preparation easy and simple to handle again.
A quality determining method for refrigerant heatstroke prevention preparation, comprises the steps:
(1) discriminating of cogongrass rhizome: take finished particle powder 3g, add chloroform 20ml, ultrasonic 30min, filter, filtrate evaporate to dryness, residue adds 0.5ml methyl alcohol makes dissolving, as need testing solution.Separately get cogongrass rhizome control medicinal material 0.1g, be made in the same way of control medicinal material solution.According to thin-layered chromatography (annex VI B) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol (10:3) for developping agent, launch, taking-up, dry, inspect under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, aobvious same color fluorescence spot.
(2) assay of glycyrrhizic acid:
The preparation of a, reference substance solution: it is appropriate that precision takes Radix Glycyrrhizae acid amide reference substance, adds 70% methyl alcohol and makes the solution of every 1ml containing 75 μ g, to obtain final product.(it is 0.9795mg that every 1mg glycyrrhizic acid amine salt amounts to glycyrrhizic acid.）
Prepared by b, need testing solution: get finished particle content appropriate, be ground into fine powder, precision takes 2.5g, adds 70% methyl alcohol 25ml, weighed weight in conical flask, ultrasonic 30 minutes, takes out, then weighs, supply the weight of less loss with 70% methyl alcohol, filters, to obtain final product.
C, chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile-water-glacial acetic acid (37:63:2.1) is mobile phase; Determined wavelength is 254nm.Number of theoretical plate calculates should be not less than 3000 by glycyrrhizic acid peak.
D, respectively accurate absorption reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product; This product should be 90% ~ 110% of labelled amount containing glycyrrhizic acid.
Computing formula:
Glycyrrhizic acid content limit × average yield (%) ÷ output (g) in glycyrrhizic acid content limit (mg/g)=Radix Glycyrrhizae inventory (g) × licorice medicinal materials in refrigerant heatstroke prevention particle
The quality determining method of above-mentioned a kind of refrigerant heatstroke prevention preparation, wherein: this product every bag contains Radix Glycyrrhizae with glycyrrhizic acid (C
42h
62o
16) meter, should 4.5mg be not less than.
The present invention compared with prior art, there is obvious beneficial effect, from above technical scheme: adopt TLC distinguish to cogongrass rhizome in refrigerant heatstroke prevention preparation, and measure the content of glycyrrhizic acid in this product, adopt high performance liquid chromatography, by experimental selection chromatographic condition repeatedly, glycyrrhizic acid and other Component seperation degree good, method precision is high, and reappearance, the recovery are all good.Therefore, method of quality control given amount provided by the invention controls the refrigerant heatstroke prevention quality of the pharmaceutical preparations, easy and simple to handle again.
Embodiment
Beneficial effect of the present invention is further illustrated below by way of test example and embodiment.
test example:
The preparation of this product: get cogongrass rhizome 300g, lophatherum gracile 300g, eleusine indica 300g, reed rhizome 300g, talcum (flying) 180g, Radix Glycyrrhizae 60g, above Six-element, boiling secondary, 2 hours first times, second time 1 hour, collecting decoction, filters, filtrate is concentrated into cream clearly, add cane sugar powder appropriate, make particle, dry, be distributed into 100 bags, obtain final product.
1, the discriminating of cogongrass rhizome:
Get finished particle content and be about 3g, add chloroform 20ml, ultrasonic 30min, filter, filtrate evaporate to dryness, residue adds 0.5ml methyl alcohol makes dissolving, as need testing solution.Separately get cogongrass rhizome control medicinal material 0.1g, be made in the same way of control medicinal material solution.According to thin-layered chromatography (annex VI B) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol (10:3) for developping agent, launch, taking-up, dry, inspect under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, aobvious same color fluorescence spot.
2, glycyrrhizic acid content measures:
The selection of content assaying method: effective constituent contained by refrigerant heatstroke prevention preparation Radix Glycyrrhizae, with reference to the assay method containing effective constituent glycyrrhizic acid in licorice medicinal materials, adopts the content of glycyrrhizic acid in high effective liquid chromatography for measuring this product.Chromatography condition is as follows, glycyrrhizic acid and other Component seperation degree good, method method precision is high, and reappearance, the recovery are all good, therefore adopts the content of glycyrrhizic acid in high effective liquid chromatography for measuring this product.
instrument and reagent:
High performance liquid chromatograph: Shimadzu LC-10AT infusion pump, SPD-10A type UV-detector, Weil-McLain dragon workstation, T-230A column oven, Yi Lite C18 post (250mm × 4.6mm, 5 μm).Chromatographic column, LIBROR AEL-160 type ten thousand/electronic analytical balance, TG332A type 100,000/analytical balance, DS-250A(frequency 50HZ) type ultrasonic cleaning instrument.
Radix Glycyrrhizae acid amide reference substance: be purchased from Products in China calibrating institute (lot number: 110731-200408), methyl alcohol is chromatographically pure, it is pure that other reagent is analysis.
System suitability test
Chromatographic column:, Yi Lite C18 post (250mm × 4.6mm, 5 μm);
Mobile phase: acetonitrile-water-glacial acetic acid (37:63:2.1); Determined wavelength: 254nm; Column temperature: 30 DEG C; Sample size: 10 μ l; Number of theoretical plate calculates should be not less than 3000 by glycyrrhizic acid peak.
Control wavelength chooses
Extracting Radix Glycyrrhizae acid amide reference substance solution carries out UV spectral scan, has maximum absorption wavelength at 254nm place, therefore selects 254nm as control wavelength.
Chromatographic condition screens
Select multiple flow phase system to carry out HPLC chromatographic condition shaker test, the results are shown in Table 1
Analyzed by above comparative test result, it is suitable that method 6 has retention time, and the features such as sample separation is effective, feminine gender is noiseless, therefore record as text.Simultaneously according to follow-up test analysis and summary, theoretical cam curve when glycyrrhizic acid can reach the minimum degree of separation 1.5 of separation in sample is 3000, and therefore the theoretical cam curve of regulation glycyrrhizic acid is not less than 3000.
the preparation of need testing solution:
In the preparation process of test sample, Extraction solvent is studied, extract with methyl alcohol, ethyl acetate, chloroform equal solvent respectively, result shows with 70% methyl alcohol as Extraction solvent, extraction effect is better, impurity peaks interference is little, and need not increase separating step, therefore selects 70% methyl alcohol as Extraction solvent.
ultrasonic time is selected
With 70% methyl alcohol as Extraction solvent, different ultrasonic time is investigated, using glycyrrhizic acid content as index, select the optimum extraction world, the results are shown in Table 2.
Test findings shows, uniform content after ultrasonic 30 minutes, therefore ultrasonic time is selected and is advisable for 30 minutes.List the method in text, that is: get this product in right amount, be ground into fine powder, precision takes 2.5g, adds 70% methyl alcohol 25ml, weighed weight in conical flask, ultrasonic 30 minutes, takes out, then weighs, supply the weight of less loss with 70% methyl alcohol, filters, to obtain final product.
the mensuration of control experiment and solvent peak
Get the negative preparation of scarce Radix Glycyrrhizae, be made in the same way of scarce Radix Glycyrrhizae negative sample solution according to need testing solution.Get solvent (70% methanol solution) respectively, lack each 10 μ l injection liquid chromatographies of Radix Glycyrrhizae negative sample solution, need testing solution and Radix Glycyrrhizae acid amide reference substance solution, test by text method, result shows: negative solution is noiseless on the position corresponding to reference substance, test sample chromatographic peak.70% methyl alcohol is without absorption peak on the position corresponding to reference substance test sample chromatographic peak, and method is feasible.
methodological study
linear relationship is investigated
Precision measures Radix Glycyrrhizae acid amide contrast solution and is mixed with 25,50,75,100,125 μ g/ml, i.e. glycyrrhizic acid concentration 24.4875,48.9750,73.4625,97.9500,122.4375 μ g/ml get 10 μ l respectively and inject high performance liquid chromatograph, carry out glycyrrhizic acid content mensuration, linear regression is carried out to glycyrrhizic acid concentration C, equation of linear regression with glycyrrhizic acid peak area A: A=14344C-6056, the range of linearity: 0.2449 ~ 1.2244 μ g, related coefficient
r=0.9998.Initial point equation A=14277C is crossed in matching,
Enter full scale equation and initial point equation is crossed in matching with minimum point (22.4875 μ g/ml) peak area generation, relative deviation is 0.62%, is less than 1%, and therefore visual full scale equation no intercept, can calculate content with one point external standard method.Experimentally result, glycyrrhizic acid is within the scope of 0.2449 ~ 1.2244 μ g, and peak area and sample size are good linear relationship.The results are shown in Table 3.
precision testprecision measures Radix Glycyrrhizae acid amide reference substance solution (75 μ g/ml), and namely glycyrrhizic acid reference substance (73.4625 μ g/ml) 10 μ l injects high performance liquid chromatograph, repeats sample introduction 5 times, with the calculated by peak area of glycyrrhizic acid, and RSD=0.76%.The results are shown in Table 4.
replica testget same lot number test sample, prepare need testing solution 5 parts according to [assay] method, with the cubage of glycyrrhizic acid, RSD=1.59%.The results are shown in Table 5.
stability testprecision measures same need testing solution, by table 4 official hour sample introduction, altogether survey 5 times, with glycyrrhizic acid calculated by peak area, result shows, test sample in 8h, without significant change before and after glycyrrhizic acid integrating peak areas value.The results are shown in Table 6.
recovery testprecision takes test sample 1.25g(6 part), precision adds newly joins 30 μ g/ml Radix Glycyrrhizae acid amide reference substance solution (namely containing glycyrrhizic acid 29.3850 μ g/ml) 25 ml, according to test sample process, to obtain final product.Carry out glycyrrhizic acid content mensuration respectively, the results are shown in table 7.
Experimental result shows, glycyrrhizic acid application of sample average recovery rate is 96.80%, RSD is 1.66%.Reach standard-required, method is feasible.
embodiment 1
A quality determining method for refrigerant heatstroke prevention preparation, comprises the following steps:
1, cogongrass rhizome is differentiated:
Take finished particle content and be about 3g, add chloroform 20ml, ultrasonic 30min, filter, filtrate evaporate to dryness, residue adds 0.5ml methyl alcohol makes dissolving, as need testing solution.Separately get cogongrass rhizome control medicinal material 0.1g, be made in the same way of control medicinal material solution.According to thin-layered chromatography (annex VI B) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol (10:3) for developping agent, launch, taking-up, dry, inspect under putting ultraviolet lamp (365nm).In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, aobvious same color fluorescence spot.
2, glycyrrhizic acid content measures:
The preparation of a, reference substance solution: precision takes Radix Glycyrrhizae acid amide reference substance 10mg, adds 70% methyl alcohol and makes the solution of every 1ml containing 75 μ g, to obtain final product.(it is 0.9795mg that every 1mg glycyrrhizic acid amine salt amounts to glycyrrhizic acid.）
Prepared by b, need testing solution: get finished particle content appropriate, be ground into fine powder, precision takes 2.5363g, adds 70% methyl alcohol 25ml in conical flask, weighed weight, ultrasonic 30 minutes, takes out, then weighs, supply the weight of less loss with 70% methyl alcohol, filter, to obtain final product.
C, chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile-water-glacial acetic acid (37:63:2.1) is mobile phase; Determined wavelength is 254nm.Number of theoretical plate calculates should be not less than 3000 by glycyrrhizic acid peak.
D, respectively accurate absorption reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, and calculates glycyrrhizic acid content (this product should be 90% ~ 110% of labelled amount containing glycyrrhizic acid), the results are shown in Table 8.
Computing formula: glycyrrhizic acid content limit × average yield (%) ÷ output (g) in glycyrrhizic acid content limit (mg/g)=Radix Glycyrrhizae inventory (g) × licorice medicinal materials in refrigerant heatstroke prevention particle.
embodiment 2-10
With embodiment 1
The results are shown in Table 8.
Glycyrrhizic acid content limit × average yield (%) ÷ output (g) in glycyrrhizic acid content limit (mg/g)=Radix Glycyrrhizae inventory (g) × licorice medicinal materials=60g × 20mg/g × 37.86% ÷ 1000g=0.45mg/g, i.e. 4.5mg/ bag in refrigerant heatstroke prevention particle.
It can thus be appreciated that this product every bag contains Radix Glycyrrhizae with glycyrrhizic acid (C
42h
62o
16) must not count and be less than 4.5mg.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, anyly do not depart from technical solution of the present invention content, the any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (3)
1. a quality determining method for refrigerant popular medicine for heat stroke, comprises the steps:
(1) discriminating of cogongrass rhizome:
(2) assay of glycyrrhizic acid:
The preparation of a, reference substance solution: it is appropriate that precision takes Radix Glycyrrhizae acid amide reference substance, adds 70% methyl alcohol and makes the solution of every 1ml containing 75 μ g, to obtain final product;
Prepared by b, need testing solution: get finished particle content appropriate, be ground into fine powder, precision takes 2.5g, adds 70% methyl alcohol 25ml, weighed weight in conical flask, ultrasonic 30 minutes, takes out, then weighs, supply the weight of less loss with 70% methyl alcohol, filters, to obtain final product;
C, chromatographic condition and system suitability: be filling agent with octadecylsilane chemically bonded silica; Acetonitrile-water-glacial acetic acid (37:63:2.1) is mobile phase; Determined wavelength is 254nm, and number of theoretical plate calculates should be not less than 3000 by glycyrrhizic acid peak;
D, respectively accurate absorption reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product; This product should be 90% ~ 110% of labelled amount containing glycyrrhizic acid.
2. the quality determining method of refrigerant heatstroke prevention preparation as claimed in claim 1, wherein the discrimination method of cogongrass rhizome is: take finished particle powder 3g, add chloroform 20ml, ultrasonic 30min, filters, filtrate evaporate to dryness, residue adds 0.5ml methyl alcohol makes dissolving, as need testing solution;
Separately get cogongrass rhizome control medicinal material 0.1g, be made in the same way of control medicinal material solution;
According to thin-layered chromatography (annex VI B) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol (10:3) for developping agent, launch, taking-up, dry, inspect under putting ultraviolet lamp (365nm);
In test sample chromatogram, on the position corresponding to control medicinal material chromatogram, aobvious same color fluorescence spot.
3. the quality determining method of a kind of refrigerant heatstroke prevention preparation as claimed in claim 1 or 2, wherein: this product every bag in glycyrrhizic acid, should be not less than 4.5mg containing Radix Glycyrrhizae.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105467059A (en) * | 2015-12-30 | 2016-04-06 | 云南理想药业有限公司 | Quality detecting method for traditional Chinese medicine composition for treating hematuresis |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101513467A (en) * | 2008-02-19 | 2009-08-26 | 赵朝群 | Method for controlling quality of dermatosis toxemia preparation |
| CN102579860A (en) * | 2011-01-17 | 2012-07-18 | 山东阿如拉药物研究开发有限公司 | Child medicament extract composition and preparation method and application thereof |
-
2015
- 2015-06-10 CN CN201510313272.1A patent/CN105004800A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101513467A (en) * | 2008-02-19 | 2009-08-26 | 赵朝群 | Method for controlling quality of dermatosis toxemia preparation |
| CN102579860A (en) * | 2011-01-17 | 2012-07-18 | 山东阿如拉药物研究开发有限公司 | Child medicament extract composition and preparation method and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| 栾海云 等: "HPLC法测定不同产地甘草中甘草酸的含量", 《滨州医学院学报》 * |
| 覃鸿恩 等: "健脑益智胶囊薄层鉴别研究", 《陕西中医学院学报》 * |
| 邢建国 等: "高效液相色谱法测定小儿止咳糖浆中甘草酸的含量", 《中药新药与临床药理》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105467059A (en) * | 2015-12-30 | 2016-04-06 | 云南理想药业有限公司 | Quality detecting method for traditional Chinese medicine composition for treating hematuresis |
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Application publication date: 20151028 |