溶剂超声提取-气相色谱-串联质谱法同时测定硅胶驱蚊手环中73种致敏性芳香剂与4种农药

Simultaneous determination of 73 fragrance allergens and 4 pesticides in silicone mosquito repellent products by ultrasonic solvent extraction combined with gas chromatography-tandem mass spectrometry

以73种致敏性芳香剂与4种农药为目标化合物,建立了硅胶驱蚊手环中致敏性芳香剂与农药同时测定的气相色谱-串联质谱(GC-MS/MS)方法。DB-17MS色谱柱分离,动态多反应监测模式(dMRM),外标法定量。采用阳性样品优化前处理条件,结果显示,以无水乙醇为提取溶剂、密闭控温超声提取可以有效提取硅胶样品中农药与致敏性芳香剂。最佳条件下,77种目标分析物在0.1~100 mg/L范围内线性良好(R^(2)>0.9920),定量限0.02~5.0 mg/kg,回收率66%~120%,相对标准偏差0.2%~9.8%。采用上述方法对14个驱蚊手环样品进行检测,共检出31种目标化合物。该方法可用于硅胶样品中致敏性芳香剂和农药高通量定向筛查。

A novel method based on ultrasonic solvent extraction and gas chromatography-tandem mass spectrometry(GC-MS/MS)was developed for simultaneous determination of 73 fragrance allergens and 4 pesticides in the silica gel products.77 analytes were separated by DB-17MS column,determined by tandem mass spectrometry in dynamic multiple reaction monitoring(d-MRM)mode,and quantified by external standard method.The GC-MS/MS parameters for 77 analytes were optimized,and the results showed that the analytes from silica gel samples could be extracted effectively using absolute ethanol as solvent under temperature controlled ultrasonic extraction.Under the optimum conditions,the linearities(R^(2)>0.9920)were obtained in the range of 0.1-100 mg/L.The limits of quantifications(LOQs)were in the range of 0.02-5.0 mg/kg with the recoveries of 66%-120% and the relative standard deviations(RSDs)of 0.2%-9.8%.Finally,14 commercial anti-mosquito silicone wristbands were analyzed,and a total of 31 analytes were found.This method was suitable for highthroughput screening of allergenic aromatic agents and pesticides in silica gel samples.