顶空单液滴微萃取-气相色谱法检测马来酸氯苯那敏中苯系物残留量

Determination of residual benzene homologues in chlorphenamine maleate by headspace single-drop microextraction-GC

目的:建立一种新的药品中残留溶剂的检测方法并对马来酸氯苯那敏中的苯、甲苯、对二甲苯进行检测。方法:采用顶空单液滴微萃取的样品处理方法分离富集苯系物,用气相色谱法检测,使用氢火焰离子化检测器,5%AT-1200+1.75%Ben-tone 34 Chromosorb W-AW 不锈钢填充柱(182cm×0.32cm),柱温80℃,汽化室温度190℃,检测器温度190℃,载气:氮气,流速25mL·min(-1)。结果:苯、甲苯和对二甲苯的检测限分别为1.3×10^(-3),1.3×10^(-3),7.8×10^(-4)μg·g^(-3);平均回收率分别为97.0%,100.2%,92.7%。结论:该方法具有装置简单、平衡时间短、平衡温度低,灵敏度高的优点。马来酸氯苯那敏中有甲苯检出但不超标。

Objective：To establish a new method for determination residual organic solvent in medicine. Benzene, toluene and p - xylene in chlorphenamine maleate was determined. Methods： Benzene homologues were concentrated by headspace single - drop microextraction and were determinated by GC. The 5% AT - 1200 ＋ 1.75% Bentone 34 Chromosorb W - AW stainless steel packed column （ 182 cm × 0. 32 cm） was used and the column temperature was 80 ℃. The flame ionization detector was used and detector temperature was 190 ℃. The injector port temperature was 190 ℃. Carrier gas was nitrogen with a flow rate of 25 mL · min^ -1 Results：The detection limits of benzene,toluene and p - xylene were 1.3 × 10 ^-3,1.3 × 10 ^-3 and 7.8 × 10^ -4 μg · g^-1 respectively. The average recoveries were 97.0% , 100.2% and 92.7% respectively. Conclusion：This method used simple apparatus, the equilibrium time was short, the equilibrium temperature was low and the sensitive was high. The toluene was found in chlorphenamine maleate, but it didn＇t exceed the standard.