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目的建立同时测定饮用水中21种半挥发性有机化合物(SVOCs)的全自动大体积固相萃取-气相色谱-串联质谱-多离子反应监测(GC-MS/MS-MRM)方法。方法取水样1 000 ml加VC除去余氯,加盐酸调节p H<2,记录加入盐酸体积(ml),再加入5.00 ml甲醇充分混匀,超声10 min,采用全自动大体积固相萃取仪装C18固相萃取柱活化、萃取、洗脱,加3 ml乙酸乙酯清洗样品瓶壁,合并入洗脱液,红外浓缩定容至1.00 ml,用GC-MS/MS-MRM对其进行定性定量测定。结果 21种SVOCs的浓度为0.000 6μg/ml~10.00μg/ml时,线性关系良好(r≥0.993 7),平均回收率为80.6%~112.8%,RSD为3.6%~9.7%,方法的检出限为0.000 04μg/L~0.002 4μg/L。结论本方法快速简便,线性范围宽,灵敏度高,检出限低,适合日常生活饮用水及水源水样品中多种SVOCs的痕量测定。
Objective To establish a fully automatic mass spectrometry (GC-MS / MS-MRM) method for the simultaneous determination of 21 semi-volatile organic compounds (SVOCs) in drinking water by gas chromatography-tandem mass spectrometry-multiple ion reaction monitoring. Methods Take 1 000 ml of water and add VC to remove residual chlorine, add hydrochloric acid to adjust p H <2, record the volume of hydrochloric acid added (ml), add 5.00 ml of methanol and mix well and sonicate for 10 min, use the automatic large volume solid phase extraction Instrument C18 solid phase extraction column activation, extraction, elution, add 3 ml of ethyl acetate to clean the wall of the sample, into the eluate, the infrared concentration to 1.00 ml, by GC-MS / MS-MRM Qualitative and quantitative determination. Results The linearity was good (r ≥ 0.993 7) with an average recovery of 80.6% ~ 112.8% and a RSD of 3.6% ~ 9.7% when the concentration of 21 SVOCs was 0.000 6μg / ml ~ 10.00μg / ml. The limit is 0.000 04 μg / L to 0.002 4 μg / L. Conclusion The method is rapid and simple, with wide linear range, high sensitivity and low detection limit. It is suitable for the determination of trace amounts of SVOCs in daily drinking water and drinking water samples.