气相色谱法测定左卡尼汀原料药中苯乙烯和二乙烯苯的残留

Determination of Styrene and Divinylbenzene in Levocarnitine by Gas Chromatography

建立左卡尼汀原料药中苯乙烯和二乙烯苯残留溶剂的气相色谱检测方法。采用HP-5毛细管色谱柱,初始柱温40℃,保持5 min,再以每分钟10℃的速率升温至180℃,维持1 min,载气为氮气,检测器为氢火焰离子化检测器(FID)。苯乙烯浓度在0.015 1~3.014μg/m L,二乙烯苯在0.100~3.011μg/m L范围内具有良好的线性;相关系数分别为0.999 7和0.999 4;平均回收率分别为111.5%和109.6%;检测限分别为0.004 5μg/m L和0.030 1μg/m L;3批左卡尼汀原料药中检测的残留溶剂均符合标准规定。该检测方法经方法学验证,适用于检测左卡尼汀原料药中苯乙烯和二乙烯苯的残留溶剂。

To establish a gas chromatographic method for determination of styrene and divinylbenzene residual solvents in evocarnitine,HP-5 capillary column was used.The initial column temperature was 40 ℃,and which was maintained for 5 min.Then the temperature was increased to 180 ℃ at the rate of 10 ℃ per minute,and the temperature was maintained for 1 min.The carrier gas was nitrogen and the detector was hydrogenflame ionization detector(FID).The concentration of styrene between 0.015 1 μg/m L to3.014 μg/m L,and that of divinylbenzene between 0.100 μg/m L to 3.011 μg/m L has a linear relationship.Correlation coefficients were 0.999 7 and 0.999 4.The average recovery was 111.5% and 109.6%.Detection limits were 0.004 5 μg/m L and0.030 1 μg/m L.All the residual solvents detected in 3 batches of levocarnitine API complied with the standards.The method can be used to detect the residual solvents of styrene and divinylbenzene in Levocarnitine.