顶空气相色谱法测定盐酸文拉法辛原料药中11种有机溶剂残留量

Determination of Residual of 11 Organic Solvents in Venlafaxine Hydrochloride Crude Drug by Headspace Gas Chromatography

目的:建立盐酸文拉法辛原料药中11种有机溶剂残留量的测定方法。方法:采用顶空气相色谱法。色谱柱为AgilentDB-624,氢火焰离子化检测器(FID)温度为250℃,进样口温度为200℃,顶空平衡温度为80℃,平衡时间为30min,载气为氮气,50%N,N-二甲基甲酰胺为溶解介质。测定3批样品中有机溶剂甲醇、乙醇、乙醚、丙酮、异丙醇、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、环己烷、甲苯的含量。结果:11种有机溶剂均能完全分离,各组分在线性范围内均呈良好线性关系(r=0.9995～0.9999),平均回收率为94.40%～102.87%,RSD≤5.27%(n=9)。3批样品中均检出异丙醇,1批检出甲苯,并符合相关要求。结论:本方法用于测定文拉法辛原料药中的有机溶剂残留,操作简便、结果可靠。

OBJECTIVE： To establish a method for the determination of 11 organic solvents in venlafaxine crude drug. METHODS： The contents of solvents were determined by Headspace GC chromatography on Agilent DB-624 column. The temperature of FID was 250 ℃, and that of injector was 200 ℃. Vial equilibrium temperature was 80 ℃, and equilibrium time was 30 min. The contents of methanol, ethanol, aether, acetone, isopropanol, dichloromethane, n-hexane, ethyl acetate, tetrahydrofuran, cyclohexane and methylbenzene were determined using nitrogen as carrier gas and 50% DMF as solvent media. RESULTS： 11 kinds of organic solvents were separated completely. Good linearity was obtained （r=0.999 5-0.999 9）. The average recovery rates were 94.40%-102.87% （RSDs≤5.27%, n=9）. Isopropanol was found in 3 batches of samples, and methylbenzene was only found in 1 batch of samples, which were all in line with the requirements. CONCLUSIONS： The method is simple, sensitive and reliable for the determination of organic solvents in venlafaxine hydrochloride crude drug.