【作者】 叶晓霞； 马娟； 杨永健；

【Author】 YE Xiao-Xia 1,2 , Ma Juan 1 , YANG Yong-Jian 2 , Jin Fang 1 1. Shanghai Institute of Pharmaceutical Industry, Shanghai 200437 2. Shanghai Institute for Food and Drug Control, Shanghai 201203

【机构】 上海医药工业研究院； 上海市食品药品检验所；

【摘要】 目的:建立气雾剂中邻苯二甲酸酯塑化剂浸出物气相-串联质谱测定方法。方法:采用GC-MS/MS,样品经DB-5MS毛细管色谱柱分离,以多反应监测模式(MRM)检测。结果:DMEP、DEEP和DBEP在40-2000ng·mL-1浓度范围内,峰面积与进样浓度的线性关系良好,其余18种邻苯二甲酸酯塑化剂在4-200ng·mL-1浓度范围内,峰面积与进样浓度的线性关系良好,线性相关系数(R2)为0.9902-0.9985。21种邻苯二甲酸酯塑化剂高、低浓度的平均加样回收率为87.5~108.3%,精密度试验的RSD均小于8%。最小检测限为0.04-4.0ng·mL-1。5批样品中均检出5种塑化剂,每罐的塑化剂总量均小于260ng。结论:此方法灵敏度高,专属性好,结果准确,可用于气雾剂中邻苯二甲酸酯塑化剂浸出物的检测。更多还原

【Abstract】 OBJECTIVE:To establish a gas chromatography tandem mass spectrometry method for the separation and detection of 21 phthalate leachables in meter dose inhaler (MDI). METHODS: After seperated by DB-5MS(30m×0.25mm×0.25μm) column,21 phthalate leachables were detected by tandem mass spectrometry method in MRM mode. RESULT: The optimized method was reliable with high sensitivity and selectivity. Calibration curves were linear with correlation coefficients R 2 >0.99, and the limits of detection were in the range of 0.04-4.0ng mL -1 . Recoveries range between 87.5% and 108.3%, and the RSD values of precision were within 8%. For the five batches of MDI analyzed, 5 phthalates (DMP, DEP, DIBP, DBP and DEHP) out of 21 phthalates were found in each sample, and the total amount of phthalates was less than 260ng canister -1 . CONCLUSION: The GC-MS /MS method established is sensitive with high selectivity and accuracy,it can be used for the determination of phthalate leachables in meter dose inhaler.更多还原