顶空气相色谱法测定药用辅料及食品添加剂硬脂富马酸钠中甲苯残留量

Determination of Residual Toluene in Sodium Stearyl Fumarate for Pharmaceutical Excipient and Food Additives by Headspace GC

目的采用顶空气相色谱法测定药用辅料及食品添加剂硬脂富马酸钠中甲苯残留量。方法采用Agilent DB-1701气相毛细管柱(0.25 mm×30 m,0.25μm),顶空进样,顶空平衡温度为110℃,顶空平衡时间为30 min;载气为N 2,流速为2.0 mL·min^(-1),分流比为20∶1,检测器为FID,进样口温度为150℃,检测器温度为250℃;采用程序升温法:起始温度30℃,保持2 min,然后以5℃/min升至40℃,保持20 min,再以20℃/min升至120℃,保持5 min,最后以30℃/min升至150℃,保持1 min;以二甲亚砜为溶剂、丁酮为内标,按内标法以峰面积计算含量。结果在1.0~203.6μg·mL^(-1)浓度范围内,甲苯与内标峰面积的比值与浓度呈良好的线性关系(r=0.9995),检测限和定量限分别为0.200μg·mL^(-1)、0.400μg·mL^(-1),精密度与重复性良好,RSD分别为0.98%、1.60%,平均回收率为99.49%;3批样品中甲苯残留含量为0.002%~0.004%。结论所建立方法准确、简便、可靠,可用于药用辅料及食品添加剂硬脂富马酸钠中甲苯残留的检测。

OBJECTIVE To establish a Headspace GC method to determine the residual toluene in sodium stearyl fumarate for pharmaceutical excipient and food additives.METHODS The method was performed on an Agilent DB-1701 column(0.25 mm×30 m,0.25μm),headspace injection,the headspace temperature was 110℃,the headspace time was 30 min.The flow rate of the carrying gas(N 2)was 2.0 mL·min^(-1),the ratio was 20∶1.The FID detector temperature was 250℃,the injector temperature was 150℃,the column temperature was changed according to the program,initial temperature was kept at 30℃for 2 min,then raised to 40℃at the rate of 5℃/min,maintained for 20 min,and then raised to 120℃at the rate of 20℃/min,maintained for 5 min,and finally raised to 150℃at the rate of 30℃/min,maintained for 1 min,dimethyl sulfoxide was used as the solvent,butanone was used as the internal standard,and the internal standard method was quantitatively determined by calculating the peak areas.RESULTS The calibration curve was linear within the range of 1.0-203.6μg·mL^(-1)(r=0.9995),the limit of detection and quantitation was 0.200μg·mL^(-1),0.400μg·mL^(-1),respectively.The precision and repeatability were good,the RSD were 0.98%and 1.60%,respectively.And the average recovery was 99.49%,the toluene content was 0.002%-0.004%in the 3 batches of samples.CONCLUSION The established method is accurate,simple,reliable,which can be used to determine the residual toluene in sodium stearyl fumarate for pharmaceutical excipient and food additives.