CN114563517A - Method for measuring glycyrrhizic acid content in children cough syrup - Google Patents
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- CN114563517A CN114563517A CN202011359284.5A CN202011359284A CN114563517A CN 114563517 A CN114563517 A CN 114563517A CN 202011359284 A CN202011359284 A CN 202011359284A CN 114563517 A CN114563517 A CN 114563517A
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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 47
- 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 title claims abstract description 39
- 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 title claims abstract description 39
- 229960004949 glycyrrhizic acid Drugs 0.000 title claims abstract description 39
- 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 title claims abstract description 39
- 239000001685 glycyrrhizic acid Substances 0.000 title claims abstract description 39
- 235000019410 glycyrrhizin Nutrition 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 32
- 206010011224 Cough Diseases 0.000 title claims abstract description 30
- 239000006188 syrup Substances 0.000 title claims abstract description 29
- 235000020357 syrup Nutrition 0.000 title claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 29
- 239000013558 reference substance Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000012085 test solution Substances 0.000 claims abstract description 12
- 238000001514 detection method Methods 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims description 19
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 14
- 239000005695 Ammonium acetate Substances 0.000 claims description 14
- 229960000583 acetic acid Drugs 0.000 claims description 14
- 229940043376 ammonium acetate Drugs 0.000 claims description 14
- 235000019257 ammonium acetate Nutrition 0.000 claims description 14
- 239000012362 glacial acetic acid Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000004811 liquid chromatography Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 239000000741 silica gel Substances 0.000 claims description 7
- 229910002027 silica gel Inorganic materials 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 238000004587 chromatography analysis Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 abstract description 36
- 239000012535 impurity Substances 0.000 abstract description 13
- 239000012074 organic phase Substances 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract description 2
- 238000013375 chromatographic separation Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 14
- 238000001228 spectrum Methods 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- VZEZONWRBFJJMZ-UHFFFAOYSA-N 3-allyl-2-[2-(diethylamino)ethoxy]benzaldehyde Chemical compound CCN(CC)CCOC1=C(CC=C)C=CC=C1C=O VZEZONWRBFJJMZ-UHFFFAOYSA-N 0.000 description 1
- 244000303040 Glycyrrhiza glabra Species 0.000 description 1
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 description 1
- 235000006751 Platycodon Nutrition 0.000 description 1
- 244000274050 Platycodon grandiflorum Species 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
- 229930006000 Sucrose Natural products 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000000954 anitussive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003172 expectorant agent Substances 0.000 description 1
- 230000003419 expectorant effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 235000011477 liquorice Nutrition 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 201000009240 nasopharyngitis Diseases 0.000 description 1
- 229930189914 platycodon Natural products 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 229940098465 tincture Drugs 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention belongs to the technical field of medicine component detection, and provides a method for determining glycyrrhizic acid content in children cough syrup. The method comprises the following steps: (1) preparing a reference substance solution; (2) preparing a test solution; (3) and (3) liquid chromatographic separation conditions. The method prolongs the peak-out time of the sample by reducing the proportion of the organic phase in the mobile phase, so that the impurity peak before the main peak in the sample map is separated from the main peak, and the method has the advantages of simple operation, high precision and high stability.
Description
Technical Field
The invention belongs to the technical field of medicine component detection, and particularly relates to a method for determining glycyrrhizic acid content in children cough syrup.
Background
The main components of the infantile cough syrup comprise liquorice fluid extract, platycodon root, orange peel tincture and ammonium chloride. The adjuvants are sucrose and sodium benzoate. Has expectorant and antitussive effects, and can be used for treating cough due to common cold in children.
When the content of glycyrrhizic acid in the children cough syrup is measured, in an experimental map of an automatic integration sample, a main component peak and an impurity peak of the sample cannot be separated, and the separation is realized by adopting a method of adjusting a slope. However, the method for adjusting the slope is not accurate, and increases workload, and the calculation is time-consuming and labor-consuming, and has a large error for fine detection.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the method for measuring the glycyrrhizic acid content in the children cough syrup, and the method prolongs the peak-appearing time of the sample by reducing the proportion of the organic phase in the mobile phase, so that the impurity peak before the main peak in the sample map is separated from the main peak, and has the advantages of simple operation, high precision and high stability.
In order to achieve the purpose, the invention adopts the following solution:
a method for measuring glycyrrhizic acid content in children cough syrup is characterized in that: the method comprises the following steps: (1) preparation of control solution: taking appropriate amount of ammonium glycyrrhizinate reference substance, precisely weighing, adding mobile phase to obtain reference substance solution containing glycyrrhizic acid, and sealing for storage; (2) preparation of a test solution: precisely measuring 1ml of the product with an internal pipette, placing in a 50ml measuring flask, washing the inner wall of the pipette with a mobile phase, adding the washing liquid into the measuring flask, adding the mobile phase to the scale, shaking up, filtering, and collecting the subsequent filtrate; (3) liquid chromatography separation conditions: theoretical plate number of separation chromatography column: not less than 2000; filling agent: octadecylsilane bond and silica gel; mobile phase: methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (59: 41: 1); detection wavelength: 250 nm.
The method for measuring the glycyrrhizic acid content in the infantile cough syrup provided by the invention has the beneficial effects that:
according to the method for determining the glycyrrhizic acid content in the children cough syrup, provided by the invention, the peak emergence time of the sample is prolonged by reducing the proportion of the organic phase in the mobile phase, so that the impurity peak and the main peak in front of the main peak in a sample map are separated, and the method is simple to operate and high in accuracy and stability.
Drawings
FIG. 1 is a graph of the peak appearance of a control solution of example 1 of the present invention;
FIG. 2 is a peak-appearing pattern of a test solution in Experimental example 1 of the present invention;
FIG. 3 is a graph of the peak appearance of a control solution of comparative example 1 of the present invention;
FIG. 4 is a peak-out plot of a test article solution of comparative example 1 of the present invention;
FIG. 5 is a peak-out plot of a test article solution of comparative example 2 of the present invention;
FIG. 6 is a peak-out plot of a test solution of comparative example 3 of the present invention;
FIG. 7 is a graph of the peak appearance of a control solution of example 2 of the present invention;
FIG. 8 is a peak-appearing graph of a test solution of lot number 180706 in example 2 of the present invention;
FIG. 9 is a graph showing the peak appearance of a test solution lot number 180707 in example 2 of the present invention;
FIG. 10 is a peak appearance of a sample solution of lot number 180708 of example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The method for determining the glycyrrhizic acid content in the infantile cough syrup provided by the embodiment of the invention is specifically explained below.
The invention provides a method for measuring glycyrrhizic acid content in children cough syrup, which comprises the following steps: (1) preparation of control solution: taking a proper amount of ammonium glycyrrhizinate reference substance, precisely weighing, adding mobile phase to obtain a reference substance solution containing glycyrrhizic acid, wherein in the embodiment, each 1ml of the reference substance solution contains 39.18 μ g of glycyrrhizic acid, and sealing for storage; (2) preparing a test solution: precisely measuring 1ml of the product with an internal pipette, placing in a 50ml measuring flask, washing the inner wall of the pipette with a mobile phase, adding the washing liquid into the measuring flask, adding the mobile phase to the scale, shaking up, filtering, and collecting the subsequent filtrate; (3) liquid chromatography separation conditions: in this example, shimadzu LC-20AT high performance liquid chromatography was used, the column diameter of the column was 4.6mm, the column length was 150mm, and the number of theoretical plates of the separation column: not less than 2000; filling agent: octadecylsilane bond and silica gel; mobile phase: methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (59: 41: 1); detection wavelength: 250nm and the column temperature is room temperature; (5) calculating the glycyrrhizic acid content in the children cough syrup: the method comprises comparing the liquid chromatogram of the sample with the liquid chromatogram of the reference substance and the retention time, and calculating the glycyrrhizic acid content of the infantile cough syrup by peak area according to standard curve method.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a method for measuring glycyrrhizic acid content in children cough syrup, which comprises the following steps: (1) preparation of control solutions: taking appropriate amount of ammonium glycyrrhizinate reference substance, precisely weighing, adding mobile phase to obtain reference substance solution containing glycyrrhizic acid, wherein each 1ml of the reference substance solution contains 39.18 μ g glycyrrhizic acid, and sealing for storage; (2) preparing a test solution: precisely measuring 1ml of the product with an internal pipette, placing in a 50ml measuring flask, washing the inner wall of the pipette with a mobile phase, adding the washing liquid into the measuring flask, adding the mobile phase to the scale, shaking up, filtering, and collecting the subsequent filtrate; (3) liquid chromatography separation conditions: adopting an Shimadzu LC-20AT high performance liquid chromatograph, wherein the column diameter of a chromatographic column is 4.6mm, the column length is 150mm, and the number of theoretical plates of the separation chromatographic column is as follows: not less than 2000; filling agent: octadecylsilane bond and silica gel; mobile phase: methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (59: 41: 1); detection wavelength: 250nm and the column temperature is room temperature.
Comparative example 1
The comparative example provides a method for determining glycyrrhizic acid content in children cough syrup, which comprises the following steps: (1) preparation of control solutions: taking appropriate amount of ammonium glycyrrhizinate reference substance, precisely weighing, adding mobile phase to obtain reference substance solution containing glycyrrhizic acid, wherein each 1ml of the reference substance solution contains 39.18 μ g glycyrrhizic acid, and sealing for storage; (2) preparation of a test solution: precisely measuring 1ml of the product with an internal pipette, placing in a 50ml measuring flask, washing the inner wall of the pipette with a mobile phase, adding the washing liquid into the measuring flask, adding the mobile phase to the scale, shaking up, filtering, and collecting the subsequent filtrate; (3) liquid chromatography separation conditions: adopting an Shimadzu LC-20AT high performance liquid chromatograph, wherein the column diameter of a chromatographic column is 4.6mm, the column length is 150mm, and the number of theoretical plates of the separation chromatographic column is as follows: not less than 2000; filling agent: octadecylsilane bond and silica gel; mobile phase: methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (65: 35: 1); detection wavelength: 250nm and the column temperature is room temperature.
Comparative example 2
The comparative example provides a method for determining glycyrrhizic acid content in children cough syrup, which comprises the following steps: (1) preparation of control solutions: taking appropriate amount of ammonium glycyrrhizinate as reference substance, precisely weighing, adding mobile phase to obtain reference substance solution containing glycyrrhizic acid, wherein each 1ml of the reference substance solution contains 39.18 μ g glycyrrhizic acid, and sealing for storage; (2) preparation of a test solution: precisely measuring 1ml of the product with an internal pipette, placing in a 50ml measuring flask, washing the inner wall of the pipette with a mobile phase, adding the washing liquid into the measuring flask, adding the mobile phase to the scale, shaking up, filtering, and collecting the subsequent filtrate; (3) liquid chromatography separation conditions: adopting an Shimadzu LC-20AT high performance liquid chromatograph, wherein the column diameter of a chromatographic column is 4.6mm, the column length is 150mm, and the number of theoretical plates of the chromatographic column is as follows: not less than 2000; filling agent: octadecylsilane bond and silica gel; mobile phase: methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (60: 40: 1); detection wavelength: 250nm and the column temperature is room temperature.
Comparative example 3
The comparative example provides a method for determining glycyrrhizic acid content in children cough syrup, which comprises the following steps: (1) preparation of control solutions: taking appropriate amount of ammonium glycyrrhizinate reference substance, precisely weighing, adding mobile phase to obtain reference substance solution containing glycyrrhizic acid, wherein each 1ml of the reference substance solution contains 39.18 μ g glycyrrhizic acid, and sealing for storage; (2) preparation of a test solution: precisely measuring 1ml of the product with an internal pipette, placing in a 50ml measuring flask, washing the inner wall of the pipette with a mobile phase, adding the washing liquid into the measuring flask, adding the mobile phase to the scale, shaking up, filtering, and collecting the subsequent filtrate; (3) liquid chromatography separation conditions: adopting an Shimadzu LC-20AT high performance liquid chromatograph, wherein the column diameter of a chromatographic column is 4.6mm, the column length is 150mm, and the number of theoretical plates of the separation chromatographic column is as follows: not less than 2000; filling agent: octadecylsilane bond and silica gel; mobile phase: methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (58: 42: 1); detection wavelength: 250nm and the column temperature is room temperature.
Experimental example 1 separation of impurity peaks from main peaks
The content of glycyrrhizic acid in the pediatric cough syrup was measured by the methods of example 1 and comparative examples 1 to 3, and the results are shown in fig. 1 to 6.
Referring to fig. 1 and 2, in example 1, the mobile phase is methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (59: 41: 1), the impurity peak and the main component peak in the sample spectrum can be separated, the separation degree can reach more than 1.5, and the peak emergence time of the reference substance and the main component peak of the sample is stable;
referring to fig. 3 and 4, in comparative example 1, the mobile phase is methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (65: 35: 1), the impurity peak and the main component peak in the sample spectrum are not completely separated, and the peaks must be accumulated by modifying the slope;
referring to FIG. 5, in comparative example 2, the mobile phase is methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (60: 40: 1), and the impurity peak and the main component peak in the sample spectrum can be separated, but the separation degree is only 1.398 (not meeting the requirement of systematic test);
referring to fig. 6, in comparative example 3, the mobile phase is methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (58: 42: 1), and the impurity peak and the main component peak in the sample spectrum can be separated, and the separation degree can reach more than 1.5. But for a longer time.
Experimental example 2 stability after separation of impurity peak from main peak
In order to determine whether the peak appearance time of the main component of the children cough syrup is stable, a mobile phase methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (59: 41: 1) is selected for 3 batches of children cough syrup (batches 180706, 180707 and 180708) to be continuously injected on another high performance liquid chromatograph, and whether the peak appearance time of the main peak of the reference substance and the main peak of the sample are stable is observed: (1) using the instrument information: name: high performance liquid chromatography (agilent); instrument numbering: j01087; the pump type: DEAB 810513; the detector model is as follows: DEABB 07202; a workstation: agilent 1260; (2) the column temperature was set at 28 ℃ and the experimental results are shown in FIGS. 7 to 10, except for the same conditions as in example 1.
Referring to fig. 7-10, experimental results show that, when the mobile phase is methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (59: 41: 1) on different equipment, the impurity peak and the main component peak in the sample spectrum can be separated, and the peak emergence time of the main component peaks of the reference sample and the sample is stable.
Therefore, in the determination of the content of glycyrrhizic acid in the children cough syrup, when the mobile phase adopts methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (59: 41: 1), the impurity peak and the main component peak in the test sample map can be completely separated, the peak-appearing time of the main component peak of the reference substance and the test sample is stable, and the peak-appearing time accords with the regulation in the fourth appendix 0512 of the 'Chinese pharmacopoeia' 2015 edition, namely, when the proportion of the mobile phase is adjusted, the allowable change range is 0.7X-1.3X when the percentage X of the small proportion component is less than or equal to 33 percent; when X is greater than 33%, the allowable variation range is X-10% to X + 10%.
In conclusion, by adopting the method for determining the glycyrrhizic acid content in the children cough syrup provided by the invention, the peak emergence time of the sample is prolonged by reducing the proportion of the organic phase in the mobile phase, so that the impurity peak before the main peak in the sample map is separated from the main peak, the operation is simple, and the accuracy rate and the stability are high.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for measuring glycyrrhizic acid content in children cough syrup is characterized in that:
(1) preparation of control solutions: taking appropriate amount of ammonium glycyrrhizinate reference substance, precisely weighing, adding mobile phase to obtain reference substance solution containing glycyrrhizic acid, and sealing for storage;
(2) preparation of a test solution: precisely measuring 1ml of the product by using an internal volume pipette, placing the product in a 50ml measuring flask, washing the inner wall of the pipette by using the mobile phase, adding a washing liquid into the measuring flask, adding the mobile phase to a scale, shaking up, filtering, and taking a subsequent filtrate to obtain the product;
(3) liquid chromatography separation conditions:
theoretical plate number of separation chromatography column: not less than 2000;
filling agent: octadecylsilane bond and silica gel;
mobile phase: methanol-0.2 mol/L ammonium acetate solution-glacial acetic acid (59: 41: 1);
detection wavelength: 250 nm.
2. The method for determining glycyrrhizic acid content in an infantile cough syrup according to claim 1, wherein: the control solution contains glycyrrhizic acid 39.18 μ g per 1 ml.
3. The method for determining glycyrrhizic acid content in an infantile cough syrup according to claim 1, wherein: the concentration of the mobile phase was 36.642. mu.g/ml.
4. The method for determining glycyrrhizic acid content in an infantile cough syrup according to claim 1, wherein: in the step (3), an Shimadzu LC-20AT high performance liquid chromatograph is adopted.
5. The method for determining glycyrrhizic acid content in an infantile cough syrup according to claim 4, wherein: in the step (3), the column diameter of the chromatographic column is 4.6mm, and the column length is 150 mm.
6. The method for determining glycyrrhizic acid content in infantile cough syrup according to claim 4, wherein: in the step (3), the column temperature is room temperature.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198619A (en) * | 2014-09-23 | 2014-12-10 | 华润三九（郴州）制药有限公司 | Quality detection method of cough syrup for children |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198619A (en) * | 2014-09-23 | 2014-12-10 | 华润三九（郴州）制药有限公司 | Quality detection method of cough syrup for children |
Non-Patent Citations (2)
| Title |
|---|
| 唐立海 等: "小儿肺咳糖浆质量标准研究", 《亚太传统医药》 * |
| 林勇杰: "HPLC测定小儿止咳糖浆中甘草酸铵的含量", 《海峡药学》 * |
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