液相色谱-三重四级杆串联质谱法快速检测水中微囊藻毒素-LR
目的 建立液相色谱-三重四级杆串联质谱法快速检测水中微囊藻毒素-LR (microcystin-LR, MC-LR)含量的分析方法。方法 将水样直接过0.45 μm滤膜, 经色谱柱XDB-C18, 以乙腈和0.1%的甲酸水为流动相, 梯度洗脱, 柱温25 ℃, 流速0.2 mL/min, 外标法定量。结果 在微囊藻毒素-LR浓度为0.2~20 μg/L的范围内呈良好的线性关系(r2=0.999)。平均加标回收率在96.8%~101.7%, 相对标准偏差为0.21%~1.80%。检出限为0.2 μg/L, 定量限为0.5 μg/L。结论 该方法快速, 准确, 适用于水样中MC-LR的检测, 为相关检测机构的监测工作提供参考。
Objective To establish a method for rapid detection of microcystin-LR (MC-LR) in water by liquid chromatography-four-stage tandem mass spectrometry. Methods The water sample was filtered through 0.45 μm membrane, then separated with a XDB-C18 column at the flow rate of 0.2 mL/min by gradient elution using acetonitrile and 0.1% formic acid water. The temperature of the column oven was maintained at 25 ℃. The result was quantitatively analyzed by external standard method. Results Microcystin-LR showed a good linear relationship in the concentration range of 0.2~20 μg/L (r2=0.999). The recoveries were 96.8%~101.7% with relative standard deviations of 0.21%~1.80%. The limit of detection was 0.2 μg/L, and the limit of quantification was 0.5 μg/L. Conclusion This method is rapid, accurate and applicable for the detection of Mc-LR in water samples, which providing reference for the monitoring work of relevant testing institutions.
标题：液相色谱-三重四级杆串联质谱法快速检测水中微囊藻毒素-LR
英文标题：Determination of microcystin-LR in water by high performance liquid chromatography coupled with triple quadrupole mass spectrometery
作者：
李芳 国家级农兽药残留及海洋生物毒素检测重点实验室
王颖 国家级农兽药残留及海洋生物毒素检测重点实验室
李献刚 国家级农兽药残留及海洋生物毒素检测重点实验室
刘栋 国家级农兽药残留及海洋生物毒素检测重点实验室
宋晓昕 国家级农兽药残留及海洋生物毒素检测重点实验室
中文关键词:微囊藻毒素,微囊藻毒素-LR,快速检测,液相色谱-三重四级杆串联质谱法,
英文关键词:microcystic toxins,microcystin-LR,rapid determination,high performance liquid chromatography coupled with triple quadrupole mass spectrometery,
发表日期：2018-06-13
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