Résumé
OBJECTIVE:To establish a method for the determination of donkey-hide gelatin in Lüjiao buxue granules. METH-ODS:Trypsin was used for enzymatic hydrolysis of donkey-hide gelatin. UPLC-QQQ/MS was adopted for the determination of don-key-hide gelatin in the preparation:Hypersil GOLD C18 column was used with mobile phase consisted of 0.1% formic acid solu-tion-acetonitrile(gradient elution)at the flow rate of 0.3 mL/min. The column temperature was 30 ℃,and sample size was 5 μL. Mass chromatography condition was that ion source was electrospray ion source;ionization mode was ESI+;multiple response mon-itoring was adopted,and characteristic molecular ion peaks of donkey-hide gelatin with mass-to-charge ratio of m/z 539.8(double charge)→ 612.4 and m/z 539.8(double charge)→ 923.8 were used as detection ion pair. Spray voltage was 3100 V;sheath gas was 20 Arb;auxiliary gas was 8 Arb;ion transfer tube temperature was 350 ℃;evaporation temperature was 350 ℃;scan mode was SRM. Collision gas was high purity argon. RESULTS:The sample size of donkey-hide gelatin ranged 20.24-2024 μg/mL(r=0.9978). The detection limit was 1%. RSDs of precision,stability and reproducibility tests were all lower than 6.0%. The charac-teristic molecular ion peaks of donkey-hide gelatin could be detected in 27 batches of samples. CONCLUSIONS:The method is spe-cific and can be used for the determination of donkey-hide gelatin in Lüjiao buxue granules.
Résumé
Objective:To establish an analytical method for the identification of donkey-hide gelatin in Fufang Ejiao Buxue gran-ule.Methods:The identification of donkey-hide gelatin in Fufang Ejiao Buxue granule was established by rapid resolution liquid chro -matography (UPLC) coupled with triple quadruple mass spectrometry (QQQ-MS).Results: The characteristic molecular peaks of donkey-hide gelatin were detected in ten batches of commercial samples .Conclusion:The present method is specific , precise and reli-able, and suitable for the identification of donkey-hide gelatin in Fufang Ejiao Buxue granule .The method provides scientific reference for the study of quality control method for gelatin ingredients in Chinese patent medicines .
Résumé
OBJECTIVE: To establish an analysis method for identification of gelatine ingredients in Chinese patent medicines. METHODS: Trypsin was used for hydrolysis of gelatins. The characteristic getalins analyses were identified by rapid resolution liquid chromatography (RRLC) coupled to triple quadruple mass spectrometry (QQQ-MS). Trypsin was used for hydrolysis of gelatins. RESULTS: The established present method was specific, precise and reliable. Gelatine ingredients as prescribed wereas detected for several samples. However, instead of gelatin ingredients as prescribed, unprescribed gelatine ingredients were as detected for some samples. CONCLUSION: The methodology validation is performed and the results are satisfied. The method can be used for identification of donkey-hide gelatin, oxhide gelatin, deer-horn glue and tortoise-shell glue in Chinese patent medicines, and provides a scientific reference for the study of quality control method of gelatin ingredients in Chinese Patent Medicines.
Résumé
Objective To investigate the compound donkey-hide gelatin syrup in reducing adverse reactions of qi-blood weakness patients caused by clozapine.Methods 132 patients from Psychiatric Hospital of Yunnan Province between January 2010 and June 2010 were randomly divided into a treatment group and a control group.Both groups were taken clozapine orally.On this basis,the treatment group was taken compound donkey-hide gelatin syrup and the control group was taken placebo syrup.After 8 weeks treatment for both groups,the PANSS,TESS,physical examination and experiment examination were observed to evaluate the clinical efficacy and safety.Results ① the total curative effect:the treatment group was 73.53％,the control group was 65.63％,showing statistical difference (x2=2.543,P＜0.05).② PANSS scores changes before and after the treatment:PANSS score at 2,4,6,8 weeks after the treatment of both groups were [(72.51 ±27.55),(60.54±24.03),(53.12± 15.27),(48.15± 11.88) in treatment group respectively,and (70.71 ±23.90),(58.89± 18.95),(53.06± 14.38),(48.98 ± 9.78) in the control group,respectively],both showing significant difference than the same group before the treatment [(103.99±39.12) in the treatment group,(99.78±34.35) in the control group] (P＜0.05).But there was no statistical significance between two groups (F=2.413,P＞0.05).③ adverse reactions:during the treatment liver function,blood cell analysis,dystonia,Parkinson's obstacle,akathisia,abnormal gastrointestinal reaction,heart rate,heart rate variability and blood pressure in the treatment group was significantly lower than the control group (x2=4.562,P＜0.05).Conclusion Compound donkey-hide gelatin syrup can effectively relieve adverse reactions in qi-blood weak psychosis patients after clozapine treatment and improve their drug tolerance.