摘要
目的:建立气质联用法测定复方肝浸膏制剂中棕榈酸和硬脂酸。方法:用甲醇超声提取复方肝浸膏片(胶囊)中的棕榈酸和硬脂酸,经气相色谱分离后,用质谱对化学成分进行确认,标准曲线法计算含量。色谱条件:HP-5MS毛细管柱(30 m×0.25 mm,0.25μm);程序升温,进样口温度250℃,载气为高纯氦气(1.0 m L·min^(-1));质谱条件:电离方式为EI,电离能量70 e V,离子源温度230℃,棕榈酸定量离子和定性离子分别为m/z 73.0和60.0、73.0、129.1、213.2,硬脂酸定量离子和定性离子分别为m/z 73.0和73.0、129.1、185.1、241.2。结果:棕榈酸和硬脂酸质量浓度分别在6.45~1 032μg·mL^(-1)和6.65~1 064μg·mL^(-1)内线性良好(r=0.999),棕榈酸和硬脂酸的平均回收率(n=9)为101.5和102.8%;不同厂家19批片剂中棕榈酸和硬脂酸的含量分别为1.2~7.8和1.3~9.5 mg·片-1,4批胶囊剂中棕榈酸和硬脂酸的含量分别为4.0~6.3和3.4~7.8 mg·粒-1。结论:经方法学验证,本方法可用于复方肝浸膏片(胶囊)中棕榈酸和硬脂酸的测定。
Objective：To establish a GC-MS analysis method for the contents determination of palmitic acid and stearic acid in compound Hepar Extractum preparations.Methods：The samples were extracted by ultrasonic wave,and separated using gas chromatography.The stearic acid and palmitic acid were confirmed by GC-MS and quantitatively analyzed with standard curve method.Chromatographic conditions：an HP-5MS capillary column（30 m×0.25 mm,0.25 μm） was used with column temperature raised by programming,the injector temperature was 250 ℃,and the carrier gas was helium（1.0 m L·min-1）.MS conditions：the ionization mode was EI,the electron energy was 70 e V,the ion source temperature was 230 ℃.The quantitative and qualitative ions were m/z 73.0 and 60.0,73.0,129.1,213.2 for palmitic acid,and m/z 73.0 and 73.0,129.1,185.1,241.2 for stearic acid were monitored.Results：The linearity ranges of palmitic acid and searic acid were 6.45-1 032 μg·mL-1（r =0.999） and 6.65-1 064 μg·mL-1（r=0.999）,respectively;the average recoveries（n=9） were 101.5% and 102.8%,respectively.19 batches of tablets and 4 batches of capsules from different manufacturers were determined,the contents of palmitic acid and stearic acid in tablets were 1.2-7.8 and 1.3-9.5 mg per tablet,and the two compounds in capsules were 4.0-6.3 and 3.4-7.8 mg per capsule,respectively.Conclusion：The established method is proved by methodology validation that it can be used for the determination of palmitic acid and stearic acid in compound Hepar Extractum tablets（capsules）.
作者
艾芸
李卓
张亚锋
王永姣
李荣
张凡
杨晓东
AI Yun LI Zhuo ZHANG Ya-feng WANG Yong-jiao LI Rong ZHANG Fan YANG Xiao-dong(Xi＇an Institute for Food and Drug Control, Xi＇ an 710054, China Laboratory of Resource Biology and Biotechnology in Western China, Ministry of Education, College of Life Science, Northwest University, Xi＇ an 710069, China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2016年第10期1875-1879,共5页
Chinese Journal of Pharmaceutical Analysis
基金
2015年国家药品计划抽验项目(项目编号110)
关键词
抗贫血药
复方肝浸膏片(胶囊)
动物原料药
棕榈酸
硬脂酸
气相色谱-质谱联用法
antianemic
compound Hepar Extractum tablets（capsules）
active pharmaceutical ingredient（API） of animal
palmitic acid
stearic acid
GC-MS
