微波辅助萃取-气相色谱/质谱-选择离子检测法同时测定纺织品中15种乙二醇醚类有机溶剂残留量

Simultaneous determination of the residual contents of15 glycol ethers in textiles by gas chromatography / mass spectrometry-selected ion monitoring technique coupled with microwave-assisted extraction

建立了一个同时测定纺织品中15种乙二醇醚类有机溶剂残留量的气质联用方法。该方法采用微波萃取技术提取样品中的待测组分,萃取溶剂为乙醇,萃取温度为100℃,萃取液直接进行气相色谱/质谱-选择离子监测法（GC/MS-SIM）测定,外标法定量。在信噪比（S/N）=3的条件下,15种乙二醇醚类有机溶剂的检出限为30-80μg/kg。在3个加标浓度水平下,15种乙二醇醚类有机溶剂的平均回收率为81.42%-92.63%,相对标准偏差为1.41%-4.94%（n=9）。该方法简便快速,灵敏度高,可完全满足纺织品中乙二醇醚类有机溶剂残留量检测工作的需要。

An effective method was established for the simultaneous determination of the residual contents of 15 glycol ethers in textiles.Residual glycol ethers in textiles were microwave-assisted extracted at 100℃, using ethanol as the extraction solvent.Then the extract was analyzed by gas chromatography/mass spectrometry-selected ion monitoring technique.The concentration of each analyte was cablirated by external standard method.At the condition of signal to noise （ S/N） of 3, the limits of detection varied from 30 to 80μg/kg for 15 glycol ethers.The spiked average recoveries changed from 81.42%to 92.63%for 15 glycol ethers under three different spiked levels while the relative standard deviation varied from 1.41%to 4.94%.The proposed method was simple, rapid, accurate and sensitive and could satisfy completely the technical demand of determination of residual glycol ethers in textiles.