中国药房2017,Vol.28Issue(15):2101-2104,4.DOI:10.6039/j.issn.1001-0408.2017.15.24
UPLC-QQQ/MS法检测驴胶补血颗粒中的阿胶
Determination of Donkey-hide Gelatin in Lüjiao Buxue Granules by UPLC-QQQ/MS
摘要
Abstract
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.关键词
超高效液相色谱-三重四极杆质谱法/驴胶补血颗粒/阿胶/特征分子离子峰Key words
UPLC-QQQ/MS/Lüjiao buxue granules/Donkey-hide gelatin/Characteristic molecular ion peak分类
医药卫生引用本文复制引用
陈鸿玉,李劲平,李文莉,丁野,孙辉,杨清,黄晓燕..UPLC-QQQ/MS法检测驴胶补血颗粒中的阿胶[J].中国药房,2017,28(15):2101-2104,4.基金项目
国家科技重大专项课题(No.2014ZX09304307) (No.2014ZX09304307)
湖南省食品药品监督管理局食品药品安全科技项目(No.湘食药科R201504) (No.湘食药科R201504)