毛细管气相色谱法测定阿莫曲坦原料药中8种有机溶剂残留量

Determination of 8 Residual Organic Solvents in Almotriptan Raw Material by Capillary GC

目的：建立测定阿莫曲坦原料药中8种有机溶剂即乙醇、乙腈、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、异丙醇与甲苯残留量的方法。方法：采用毛细管气相色谱法。色谱柱为AgilentDB-5毛细管柱，柱温采取程序升温，氢火焰离子化检测器，检测器温度为250℃，载气为高纯N2，进样口温度为200℃，顶空进样，平衡条件为100℃、30min。结果：8种有机溶剂在各自的检测质量浓度范围内线性关系良好（r为0．9996～0．9999），平均回收率为99．8％～100．8％（RSD为0．87％～2．11％，n=3），定量限为0．09～0．54ng，检测限为0．03～0．18ng。3批样品中只检出异丙醇。结论：建立的方法操作简便，可对阿莫曲坦原料药中残留的8种有机溶剂进行有效控制。

OBJECTIVE： To establish the method for the determination of 8 residual organic solvents including ethanol, acetonitrile, dichlormethane, n-hexane, acetic ether, tetrahydrofuran, isopropanol and methylbenzene in almotriptan raw material. METHODS： Capillary GC was used. The determination was performed on Agilent DB-5 capillary column, by temperature programming; the flame ionization detector was used with temperature of 250 ℃. High-purity N2 was used as carrier gas, and injector temperature was 200 ℃; in headspace sampling, equilibrium condition was 100 ℃ and 30 min. RESULTS： There was good linear relationship between the concentrations of 8 organic solvents and absorption area value （r were 0.999 6-0.999 9） with average recovery of 99.8%-100.8% （RSD were 0.87%- 2.11%, n=3）. The limits of quantification were 0.09-0.54 ng, and that of detection were 0.03-0.18 ng. Only isopropanol was detected in 3 batches of samples. CONCLUSIONS： Established method is simple and can be used for the quality control of 8 organic solvents in almotriptan raw material.