超高效液相色谱–串联质谱法测定饮用水中微囊藻毒素

建立饮用水中微囊藻毒素(MC–RR,MC–LR)的超高效液相色谱–串联质谱检测方法。样品经PVDF针式过滤头过滤后直接进样,采用喷雾正离子源(ESI~+)和多重反应监测模式(MRM)测定。MC–RR的质量浓度在0.02~10.00μg/L范围内与色谱峰面积呈良好的线性,线性相关系数r~2=0.998 9,检出限为0.096μg/L,测定结果的相对标准偏差为6.6%~9.1%(n=7),加标回收率为99.0%~103.0%。MC–LR的质量浓度在0.1~20μg/L范围内与色谱峰面积呈良好的线性,线性相关系数r~2=0.999 2,检出限为0.188μg/L,测定结果的相对标准偏差为4.3%~10.0%(n=7),加标回收率为93.0%~114.0%。该方法灵敏度高、重现性好,可用于饮用水中微囊藻毒素的检测。

Determination of Microcystin in Drinking Water by UPLC-MS-MS

A method was established for the determination of microcystin (MC-RR,MC-LR) in drinking water by high performance liquid chromatography tandem mass spectrometry.The sample was filtered by PVDF needle type filter,then sampled directly and detected with eleetrospray positive ion source(ESI+) and multiple reaction monitoring mode (MRM).The concentration of MC-RR was linear with chromatographic peak area in the range of 0.02-10.00 μ g/L with the correlation coefficient (r2) of 0.998 9,the detection limit was 0.096 μ g / L,the relative standard deviation of detection results was 6.6％-9.1％(n=7),and the addition recoveries was 99.0％-103.0％.The concentration of MC-LR was linear with chromatographic peak area in the range of 0.1-20 μ g / L with the correlation coefficient (r2) of 0.999 2,the detection limit was 0.188 μ g / L,the relative standard deviation of detection results was 4.3％-10.0％ (n=7),and the addition recoveries was 93.0％-114.0％.The method has higher sensitivity and good reproducibility,it is suitable for the determination of microcystin (MC-RR,MCLR) in drinking water.