建立了高效液相色谱-离子阱二级质谱法同时测定饮用水中内分泌干扰物、农药残留和丙烯酰胺等15种痕量有机污染物的方法。250mL水样先用C18固相萃取柱富集,经梯度洗脱液相色谱分离,采用时间分段的方法确定各组分质谱检测条件,利用离子阱二级质谱进行测定。所检测的15种有机污染物定量线性关系良好,相关系数为0.9975~0.9998,检测限在0.2~20ng/L之间。在低、中、高3个不同加标水平下,实际水样的加标回收率为75.1%~99.5%,相对标准偏差为4.6%~12.3%。该方法成功用于5种不同来源饮用水样的检测,获得了满意结果。
A high performance liquid chromatography-ion trap mass /mass spectrometric method had been developed for the simultaneous determination of 15 trace organic pollutants including endocrine disrupting compounds,pesticide residues and acrylamide in drinking water.The procedure includes an off-line solid-phase extraction of 250mL water samples with a C18 cartridge,followed by liquid chromatographic separation with gradient elution,and then detection by ion trap mass /mass spectrometry in consecutive time segments corresponding to the elution window of the different analytes.Good linear range was obtained for all analytes with the correlation coefficients of 0.9975 ~ 0.9998,and the detection limits were 0.2 ~ 20ng /L.The average recoveries of 15 analytes in spiked tap water samples with low,medium and high levels ranged from 75.1% ~ 99.5%,and the relative standard deviations were between 4.6% ~ 12.3% 。 The presented method has been applied to the analysis of 5 kinds of drinking water samples with satisfactory results.