毛细管气相色谱法测定米铂原料药中5种有机溶剂残留量

目的：建立测定米铂原料药中乙醇、丙酮、异丙醇、乙腈与二氯甲烷残留量的方法。方法：采用毛细管气相色谱法，色谱柱为Agilent~管柱（6％氰丙基苯基-94％二甲基硅氧烷为固定液），柱温采用程序升温；氢火焰离子化检测器温度为250℃；载气为高纯Nz；进样口温度为200oC，分流比为20：1；采用顸空进样法测定，加热温度和时间分别为90℃、30min。结果：乙醇、丙酮、异丙醇、乙腈与二氯甲烷在各自的检测质量浓度范围内线性关系良好，相关系数均≥0．9998，平均回收率为99．1％～102．9％（RSD≤2．03％，n=3）；3批样品中只检出乙醇。结论：建立的方法快速、灵敏，可用于米铂原料药中有机溶剂残留量的测定。

Content Determination of 5 Kinds of Residual Organic Solvents in Miriplatin Raw Material by Capillary GC

OBJECTIVE： To establish the method for the determination of residual amount of alcohol, acetone, isopropanol, acetonitrile and dichlormethane in miriplatin. METHODS： Capillary GC was adopted. The determination was performed on Agilent capillary column （6% cyanopropyl phenyl -94%dimethyl siloxane as stationary liquid） by temperature programming. The tempera- ture of flame ionization detector was 250 % using high-purity nitrogen as carrier gas. The temperature of injector was 200 ~C. The split ratio was 20 ： 1. Headspace sampling was adopted, and heating temperature and time were 90 ℃ and 30 min. RESULTS： There was a good linear relationship of the concentrations of alcohol, acetone, isopropanol, acetonitrile and dichlormethane with correlation coefficient≥0.999 8. Average recoveries were 99.1%-102.9% （RSD≤2.03 %, n=3）. Only the alcohol was detected in 3 batches of samples. CONCLUSIONS ： The established method is rapid and sensitive, and it is suitable for the determination of re- sidual organic solvent in miriplatin raw material.