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2.2.3 glycine, DL-methionine and glycine were taken failure test, DL-Methionine 6 mg reference standard set 10 ml volumetric flask, distilled water to volume, as the stock solution. 1ml stock solution were taken to 10 ml volumetric flask, and then were added to 1 mol · L-1 of HCl solution, 1 mol · L-1 of the NaOH solution and 30% H2O2 solution of 1 ml, 80 ℃ water bath 30 min, adjusted pH to neutral, depending on conditions treated derivative [5], which was glycine, DL-methionine reference standard acid, alkali, strong oxidizing destruction of the sample; were taken glycine, DL-methionine reference standard amount, set the oven 130 ℃ 1.5 h , dissolved in distilled water, the derivative, the system may damage the sample temperature. Samples were taken for determination of the damage. The results shown in Figure 4.
2.2 specificity study
Glycyrrhizin in the determination of related substances

Of: Tin Chun Li Haiyun high Xiaoli Tian Qi

2.3.1 Glycyrrhetate experimental precision linear relationship between ammonium glycyrrhizic acid monoammonium weighed amount of reference substance, preparation of 50% methanol concentration 0.101,1.012,5.06,Tory Burch Shoes 9eSHtory burch sale possibilities,50.6,101.2 , 303.6,Tory Burch On Sale 2mYmTory Burch,Tory Burch Shoes,506 μg · ml-1 of the series of standard solution, 20 μl sample were determined to take to the concentration of the peak area of ​​regression, the regression equation: Y = 15 311X-5 888, r = 0.9999, linear range of 0.101 ~ 506 μg · ml-1.

Figure 1 HPLC ammonium Glycyrrhetate Figure

2.3.2 glycine, DL-methionine linear relationship between the experiments were accurately weighed glycine, DL-methionine appropriate reference substance, were made into about 600 μg · ml-1 solution, take this solution After the amount of derivatives [5], dubbed the glycine concentration 0.014,0.97,24.19,72.58,96.77 μg · ml-1 of the reference solution, DL-methionine concentration 0.048,0.48,9.50,47.52,95.04,158.4,237.6 μg · ml-1 of the standard solutions, sample measurements to concentration on the peak area of ​​regression, the regression equation. Glycine: Y = 132 572X-4 129.4,MBT footwear, r = 0.999 8, the linear range of 0.014 ~ 96.77 μg · ml-1; DL-methionine: Y = 71 699X-84 781, r = 0.999 7, the linear range of 0.048 ~ 237.6 μg · ml-1.

Monoammonium glycyrrhizin (Pharmaceutical and Biological Products, batch number 11073-200513); glycine (Pharmaceutical and Biological Products, batch 140689.200401), DL-methionine (Sigma Corporation, approved No. 0,580,123, the content> 99%). Glycyrrhizin tablets (Xinjiang special Fung Pharmaceutical Co., Ltd., batch number 20070513,20070514,Tory Burch Boots,mulberry bags sale,20070515). Glycyrrhizin tablets (brand name: the United States can; Pharmaceutical Co., Ltd. originated in Japan Camino production, batch number 06130).

The figure shows, the chromatographic conditions can be Glycyrrhetate ammonium, glycine, DL-methionine under the conditions of the destruction of the main component peak of degradation products can be completely separated, segregated Pharmacopoeia requirements, does not affect Determination of the main drug.

2.2.1 Experimental access to the mobile phase solvent blank made of the blank solution, according to the following
2 Methods and results
Abstract: ObjectiveTo develop a reversed-HPLC method (PDA) for simultaneous determination of related substances of three major components in compound glycyrrhizin tablet.MethodsA C18 column was used with the mobile phase of 0.025 mol · m l-1 NaAC solution (pH 3.5) - acetonitrile (59:41) and the detection wavelength was at 251 nm and 360 nm. ResultsResolution and detectable sensitivity of each constituent in samples satisfied the detection demand of related substance. The LOD of glycyrrhizin , glycine, DL-methionine were 2.02 ng, 0.28 ng and 0.96 ng, respectively. ConclusionThe method is sensitive, accurate, simple and specific. It can be used as a reliable method for the quality control of compound glycyrrhizin tablet.
Key words glycyrrhizin ammonium salt tablets Glycyrrhetate DL-methionine glycine HPLC related substances
2.1 Chromatographic conditions [5] Shimadzu VD-ODS C18 column (250 mm × 4.6 mm, 5 μm),nike dunks,Tory Burch, mobile phase 0.025 mol · L-1 sodium acetate solution (pH 3.5 ) - acetonitrile (59:41); flow rate of 1 ml · min-1; column temperature 35 ℃; detection wavelength λ glycyrrhizic acid = 251 nm, λ amino acids = 360 nm; injection volume was 20 μl. Accessories solution to the blank, standard solution and sample solution into the sample were determined. Glycyrrhetate retention time of ammonium in 5.2 min, chromatography shown in Figure 1; glycine, DL-methionine and the retention time of derivatized DNFB were 4.3,6.7 and 5.6 min, the chromatogram shown in Figure 2. Number of theoretical plates, respectively Glycyrrhetate ammonium, glycine, DL-methionine were higher than 3000 meter peaks, all the main components and impurities were more than 1.5.
Key words: Compound glycyrrhizin tablets; Glycyrrhizin; Glycine; DL-methionine; Related substance; RP-HPLC
2.3 linear relationship
Glycyrrhizin tablets (brand name: the United States can) is a single-ammonium glycyrrhizic acid, glycine,Tory Burch On Sale, DL-methionine compound formed in 1948 in Japan, is mainly for the treatment of chronic liver disease, abnormal liver function improved, but also for the treatment of allergic reactions (such as rash, urticaria, drug rash), alopecia areata, systemic lupus erythematosus and infectious atypical pneumonia, efficacy, clinical application has been for many years [ ],[Licorice from traditional Chinese herbal medicines can be extracted acid, salt can be prepared by then had Glycyrrhetate ammonium salt, has long been widely used in pharmaceutical, food and cosmetics and other fields and other uses of the clinical safety testing has been received FDA approval [3], but the provisions of national standards in a single ammonium salt of glycyrrhizic acid content of 73.0% [4],tory burch sale, indicating that single-ammonium glycyrrhizic acid related substances in the drug substance content. To ensure the quality of the preparation and between consistency and safety, visit the related substances test.

Shimadzu SCL-20AVP high performance liquid chromatograph, SPD-M20 diode array detector (PDA), LC-solution Shimadzu chromatography workstation; THZ-82-type constant temperature bath oscillator ( Industry and Trade Co., Ltd. Shanghai often look); BP211D Precision Balance (Germany Sartorius).
Abstract aims to establish simultaneous determination of glycyrrhizin tablets three principal components related substances in RP-HPLC (diode array detector), to control the quality . Methods The C18 column using 0.025 mol · L-1 sodium acetate solution (pH 3.5) - acetonitrile (59:41) elution, detection wavelength of 251,360 nm. Results of the principal components in the sample with the substance of separation and the detection sensitivity can be determined to meet the requirements of single-ammonium glycyrrhizic acid, glycine, DL-methionine the lowest detection limits were 2.02,0.28,0.96 ng. Conclusion The method is sensitive, accurate,Tory Burch Handbags Make Shopping Fun Again defrenteproespelho.com, simple, specific, and can be used as an effective quality control of the preparation method.
Chromatography pure acetonitrile, 2,4 - dinitrofluorobenzene (DNFB), acetic acid, anhydrous sodium acetate, sodium bicarbonate, sodium hydroxide were of analytical grade. Water double distilled water.
1 instrument and reagent
2.2.2 Glycyrrhetate experiments take damage ammonium Ammonium Glycyrrhizin set reference substance 5 mg 10 ml flask, 50% methanol solution to volume, 1 ml of this solution were taken to 5 ml volumetric flask, and then were added to 1 mol · L-1 of HCl solution, 1 mol · L-1 of the NaOH solution and 30% H2O2 solution of 1.0 ml, 80 ℃ water bath 30 min, adjusted to neutral pH, 50 % methanol and diluted to the mark, that was one of glycyrrhizic acid ammonium salt of acid, alkali, strong oxidizing destruction of the sample; take Glycyrrhetate ammonium amount, set the oven 130 ℃ 1.5 h, with 50% methanol solution at constant volume heat damage to samples obtained . Samples were taken for determination of the damage. The results shown in Figure 3.
A-blank sample b-glycyrrhizic acid monoammonium reference substance for the test product c-1. Glycyrrhizic acid mono-ammonium salt
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