顶空毛细管气相色谱法测定伏立诺他原料药中有机溶剂残留量  

Quantitative determination of residual organic solvents in crude drug of vorinostat by headspace-capillary gas chromatography

作　　者：黄斌[1] 史群志[2] 李景[1] 朱小华 何作瑜[1] 

机构地区：[1]遵义医学院第五附属(珠海)医院,广东珠海519000 [2]长沙市中心医院药学部,长沙410004 [3]南京天海医药科技有限公司,南京210018

出　　处：《中南药学》2018年第1期100-103,共4页Central South Pharmacy

基　　金：贵州省科学技术基金项目(No.黔科合LH字[2014]7560号)

摘　　要：目的建立顶空毛细管气相色谱法测定伏立诺他原料药中有机溶剂残留。方法色谱柱为DB-5石英毛细管柱(30 m×0.53 mm×3μm),载气为氮气,检测器为氢火焰离子化检测器,以程序升温方式使伏立诺他中石油醚(其主要组分)、甲醇、乙醇、乙腈、乙酸乙酯、四氢呋喃达到完全分离;并采用GC-MS对石油醚(60~90℃)中主要组分进行分析鉴定,其主要组分为2-甲基戊烷、3-甲基戊烷和正己烷,这3个主要组分的限度按正己烷残留量的限度试验。结果 8种有机溶剂在相应的检测范围内与峰面积线性关系良好,回收试验符合要求。伏立诺他原料药中除了甲醇和乙醇外,其他有机溶剂均未检出。结论该方法灵敏、准确,适用于伏立诺他原料药质量控制中的有机残留溶剂检查。Objective To establish a headspace-capillary gas chromatography （GC） method to determine the residual organic solvents in vorinostat. Methods A column DB-5 capillary （30 m ×0.53 mm×3μm） was adopted, and nitrogen was the carrier gas. Petroleum ether, methanol, ethanol, acetonitrile, ethyl acetate, and tetrahydrofuran were completely separated through gradient temperature method with a flame ionization detector. The 3 main components in petroleum ether （60 - 90 ℃ ）, namely 2-methylpentane, 3-methylpentane and n-hexane, which were identified by GC-MS, and were tested according to the residue limitation ofn-hexane. Results Eight residual organic solvents were completely separated, presenting a good linearity and good recovery rate. Conclusion The proposed method meets the detecting demand in accuracy and sensitivity, and it is suitable for the determination of residual organic solvents in vorinostat.

关 键 词：石油醚 有机溶剂残留量 气相色谱法 伏立诺他 

分 类 号：R917[医药卫生—药物分析学]