超声萃取-气相色谱-串联质谱法测定纺织品中硫酸二甲酯和硫酸二乙酯的残留量

Simultaneous determination of residual dimethyl sulfate and diethyl sulfate in textiles by gas chromatography-tandem mass spectrometry coupled with ultrasonic extraction

建立了一个同时测定纺织品中硫酸二甲酯(DMS)和硫酸二乙酯(DES)残留量的气相色谱-串联质谱(GCMS/MS)方法,该方法以甲醇作为萃取溶剂,40℃下超声萃取纺织品中的DMS和DES,萃取液经滤膜0.22μm过滤后直接进行GC-MS/MS测定,外标法定量。在信噪比(S/N)=10的条件下,DMS和DES的定量限分别为10、5μg/kg。在三个加标水平下,该方法的加标平均回收率为82.2~95.8%,相对标准偏差(RSD)为1.2~6.6%(n=9)。该方法简便快捷,灵敏度高,定量限低,可完全满足纺织品中DMS和DES残留量检测的工作要求。

An effective method was established for the simultaneous determination of residual dimethyl sulfate （DMS） and diethyl sulfate （DES） in textiles by gas chromatography-tandem mass spectrometry （GC/MS-MS） technique. DMS and DES in textiles were ultrasonically extracted at 40 ℃, using methanol as the extraction solvent. The extracts were analyzed by gas chromatography-tandem mass spectrometry. The concentration of DMS and DES was calibrated by external standard method. The limit of quantitation （LOQ） was 10μg/kg and 5μg/kg for DMS and DES, respectively, at the condition of sig- nal to noise （S/N） of 10. The spiked average recoveries changed from 82.2 % to 95.8 % under three different spiked levels while the relative standard deviation （RSD） varied from 1.2 % to 6.6 %. The proposed method was simple, rapid and accu- rate, and the limits of quantification is low. It was applicable to the determination of residual dimethyl sulfate and diethyl sulfate in textiles, and provided a reference for the relevant testing standard.