GC法测定注射用丙戊酸钠中的2-甲基戊酸  

Determination of 2-methylvaleric acid in the sodium valproate for injection by GC

作　　者：杨怡晨 杨琴 孙样 邓海星 钱广生[1] YANG Yichen;YANG Qin;SUN Yang;DENG Haixing;QIAN Guangsheng(West China School of Pharmacy,Sichuan University,Chengdu,Sichuan,610041 P.R.China;Central Nervous System Drug Key Laboratory of Sichuan Province,Shichuan Credit Pharmaceutical Co.,Ltd.,Luzhou,Sichuan,646100 P.R.China)

机构地区：[1]四川大学华西药学院,四川成都610041 [2]四川科瑞德制药股份有限公司厅市共建中枢神经系统药物四川省重点实验室,四川泸州646100

出　　处：《华西药学杂志》2021年第5期570-573,共4页West China Journal of Pharmaceutical Sciences

摘　　要：目的采用气相色谱法测定注射用丙戊酸钠中2-甲基戊酸的含量。方法样品依次用水溶解、稀硫酸酸化、正庚烷萃取;采用DB-FFAP色谱柱(30 m×0.53 mm, 1.50μm),程序升温,火焰离子化检测器检测,不分流进样;以苯乙酸乙酯为内标物,按内标法以峰面积计算含量。结果 0.5245~10.49μg·mL^(-1) 2-甲基戊酸呈良好的线性关系(r=0.9992),定量限为0.3μg·mL^(-1),平均回收率为101.1%,RSD=3.22%。结论所用方法准确度好、专属性强,可以用于注射用丙戊酸钠中2-甲基戊酸的含量测定。OBJECTIVE To determine the content of 2-methylvaleric acid in sodium valproate for injection by Gas chromatography.METHODS The samples were dissolved in water, then acidified with dilute sulfuric acid and extracted with n-heptane successively.The GC column was DB-FFAP(30 m×0.53 mm, 1.50 μm) column, programmed rise temperature.The detector was flame ionization detector(FID) and samples were injected by splitless inlet.Ethyl phenylacetate was used as the internal standard, and the content of 2-methylvaleric acid was calculated by the peak area according to the internal standard method.RESULTS 2-methylvaleric acid showed a good linear relationship in the range of 0.5245-10.49 μg·mL^(-1)(r=0.9992).The limit of quantitation was 0.3 μg·mL^(-1) and the average recovery was 101.1% with the RSD of 3.22%.CONCLUSION The method is accurate and specific, and can be used for the determination of 2-methylvaleric acid in the sodium valproate for injection.

关 键 词：气相色谱法 注射用丙戊酸钠 2-甲基戊酸 程序升温 内标法 苯乙酸乙酯 不分流 含量测定 

分 类 号：R917[医药卫生—药物分析学]