分散固相萃取-增强型去除脂质-LC-MS/MS法测定衣物洗涤剂中的马来酸二乙酯

Determination of diethyl maleate in laundry detergent by dispersed solid phase extraction-enhanced lipid removal-liquid chromatography-tandem mass spectrometry

建立以分散固相萃取-增强型去除脂质(QuEChERS EMR-Lipid)为前处理方法,液相色谱-串联质谱法测定衣物洗涤剂中马来酸二乙酯含量的方法。样品在60℃水浴中经乙腈超声提取,以QuEChERS EMR-Lipid净化管快速净化,用液相色谱-串联质谱法分析,色谱峰外标法定量。马来酸二乙酯的质量浓度在0.5~100.0μg/L范围内与色谱峰面积成良好的线性关系,线性相关系数均大于0.9996。样品加标回收率为92.7%~98.2%。对样品进行6次重复测定,测定结果的相对标准偏差为1.2%~4.6%。该方法前处理简单、快捷,灵敏度高,定性定量准确,可用于衣物洗涤剂中马来酸二乙酯含量的快速检测。

The method with dispersed solid phase extraction-enhanced lipid removal(QuEChERS EMR-Lipid)method pretreament for the determination of diethyl maleate in laundry detergent by liquid chromatography-tandem mass spectrometry(LC-MS/MS)was established.Sample was ultrasonic extracted in 60℃by acetonitrile,and purified by QuEChERS EMR-Lipid purification pipe,then detected by LC-MS/MS with external standard method for quantification.The mass concentration of diethyl maleate in the range of 0.5-100.0μg/L had good linear relationship with chromatographic peak area,and the linear correlation coefficients were all more than 0.9996.The recovery was 92.7%-98.2%.The relative standard deviation of determination results was 1.2%-4.6%(n=6).The method is simple,rapid,sensitive and accurate in both quantitation and qualitation,which is suitable for the routine determination of diethyl maleate in laundry detergent.