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目的建立饮用水中9种农药残留和微囊藻毒素LR的在线固相萃-取液相色谱-串联质谱(online SPE LC-MS/MS)的检测方法。方法采用在线固相萃取技术,水样经HRP SPE柱富集,HSS T3高效液相色谱柱分离,乙腈和甲酸水梯度洗脱,分别用三重四极杆串联质谱和飞行时间质谱检测,ESI正离子模式下采集数据,外标法定量。结果 10种目标化合物的定量限远低于我国生活饮用水卫生标准的限量要求,其中飞行时间质谱法的LOQ为0.08～0.40μg/L,三重四级杆质谱法的LOQ为0.01～0.19μg/L。3个加标水平下(0.1、0.2、1倍的标准限量),10种目标物的加标回收率为66.5%～130.3%,相对标准偏差为0.8%～14.5%。结论该方法快速、简单、灵敏度高,适用于饮用水中有关农药残留和藻毒素的同时检测。
Objective To establish an online SPE-MS / MS method for the determination of nine pesticide residues and microcystin LR in drinking water. Methods Solid-phase extraction (SPE) was used. Water samples were concentrated by HRP SPE, separated by HSS T3 and eluted with gradient of acetonitrile and formic acid. The ESI-MS was detected by triple quadrupole tandem mass spectrometry and time of flight mass spectrometry. Ion mode data acquisition, external standard method. Results The limit of quantitation of 10 target compounds was much lower than the limit of the drinking water standard in China. The LOQ was 0.08 ~ 0.40μg / L in time of flight mass spectrometry, and the LOQ in triple quadrupole mass spectrometry was 0.01 ~ 0.19μg / L. The spiked recoveries of 10 target species ranged from 66.5% to 130.3% with relative standard deviations of 0.8% to 14.5% at three spiked levels (0.1, 0.2 and 1 times the standard limit). Conclusion The method is rapid, simple and sensitive. It is suitable for the simultaneous detection of pesticide residues and algal toxins in drinking water.