建立盘式固相萃取–超高效液相色谱–串联质谱(UPLC–MS–MS)快速测定环境水样中3种微囊藻毒素(MCs)的方法。环境水样经过盘式固相萃取柱净化，采用Waters BEH C18色谱小柱，以乙腈–0.2%甲酸水溶液为流动相，梯度洗脱分离后，UPLC–MS–MS多级监测正离子模式下外标法进行定性定量分析。3种微囊藻毒素在0.05～10.0µg／L范围内呈现良好线性关系，相关系数均大于0.9994，方法检出限为0.02 ng／L。对同一环境样品进行0.1，1.0，5.0µg／L 3种浓度的加标回收试验，平均回收率为82.8%～108.8%，测定结果的相对标准偏差为2.1%～10.1%(n=6)。该方法快速、灵敏、准确，可有效应用于环境水样中微囊藻毒素的监测。%A rapid determination of three kinds of microcystin algae toxins(MCs) in environmental water samples method by using disk SPE–ultra high performance liquid chromatography–tandem mass spectrometry (UPLC–MS–MS) was established. Environmental water samples was extracted by disc solid–phase extraction column(C18), three kinds of MCs was separated by Waters BEH C18 chromatographic column with acetonitrile–0.2% formic acid solution as mobile phase, gradient elution separation, UPLC–MS–MS multi–stage monitoring mode (MRM) under the external standard method was used for quantitative analysis. Three kinds of MCs in the range of 0.05–10.0 µg/L showed good linear relation, the correlation coefficient were more than 0.999 4, the method detection limit was 0.02 ng/L. Under 0.1, 1.0, 5.0 µg/L standard addition for the same environmental samples, the average recovery was 82.8%–108.8%. The relative standard deviation of determination results was 2.1%–10.1%(n=6). This method is rapid, sensitive and accurate, it can be effectively applied monitoring of algal toxins in environmental water samples.
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