直接进样-超高效液相色谱-串联质谱法测定生活饮用水中的微囊藻毒素  

Determination of microcystins in drinking water by ultra high performance liquid chromatography-triple quadrupole mass spectrometry

作　　者：杨雪丽[1] 王猛[1] 肖潇[1] 王庆国[1] 王冉冉[1] YANG Xue-li;WANG Meng;XIAO Xiao;WANG Qing-guo;WANG Ran-ran(Xinjiang Uygur Autonomous Regional Center for Disease Control and Prevention,Urumchi,Xinjiang 830001,China)

机构地区：[1]新疆维吾尔自治区疾病预防控制中心,新疆乌鲁木齐830001

出　　处：《中国卫生检验杂志》2020年第7期805-807,816,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的为提高实验室水质检测效率,建立直接进样-超高效液相色谱-串联质谱法测定生活饮用水中微囊藻毒素-LR(MC-LR)与微囊藻毒素-RR(MC-RR)的分析方法。方法考察了不同滤膜对实验结果的影响,最终选取了聚丙烯滤膜(GHP)滤膜。水样经0.22μm GHP微孔滤膜过滤后直接上机,经ACQUITY UPLC BETH C18柱(100 mm×2.1 mm,1.7μm)分离,在电喷雾正离子模式(ESI+)下电离,多反应监测模式(MRM)进行检测,外标法定量。结果2种微囊藻毒素的浓度与其峰面积在一定浓度范围内均呈现良好的线性关系(r≥0.9998),微囊藻毒素LR与MR方法检出限分别为0.02μg/L、0.05μg/L。低、中、高3个浓度加标样品的回收率相对标准偏差为3.1%~7.2%(n=6),实际样品加标平均回收率为88.3%~106.1%。结论此方法具有样品处理简单、灵敏度高、干扰小、分析速度快等优点,适用于生活饮用水中微囊藻毒素LR与MR的测定。Objective To improve the detection efficiency,a method of rapid and simultaneous determination of MC-LR and MC-RR in drinking water by ultra high performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS)method combined with direct injection was established in this study.Methods The influence of different kinds of microporous membrane on the experimental results was investigated,GHP microporous membrane was finally selected.The water samples were filtered by 0.22μm microporous membrane,then separated by Waters ACQUITY UPLC BETH C18 column(100 mm×2.1 mm,1.7μm).The samples were detected by multi-reaction monitoring(MRM)mode with positive electro spray ionization(ESI+).The microcystins were quantified by external standard method.Results Microcystins showed good linearity in suitable ranges with correlation coefficients(r)were greater than 0.9998.The detection limits of MC-LR and MC-RR were 0.02μg/L and 0.05μg/L.The average recoveries of MC-LR and MC-RR were with 88.3%-106.1%,with RSD of 3.1%-7.2%(n=6).Conclusion This method is accurate and rapid,easy to operate for MC-LR and MC-RR analysis in drinking water.

关 键 词：直接进样 液质联用 微囊藻毒素 生活饮用水 

分 类 号：O657.63[理学—分析化学]