高效液相色谱-串联质谱联用法测定饮用水中5种微囊藻毒素

目的建立液相色谱-串联质谱法同时测定饮用水中5种微囊藻毒素(MC-LR、MC-LW、MC-RR、MC-LF、MC-YR)检测的方法。方法采用直接进样方式,用高效液相色谱-串联质谱(HPLC/MS/MS)测定饮用水和水源水中的微囊藻毒素。水样经0.22μm微孔滤膜过滤,采用HPLC/MS/MS电喷雾电离阳离子(ESI+),多反应监测(MRM)模式检测,外标法定量。结果方法的线性范围为0.5～50.0μg/L,线性相关系数0.9994～1.0000,检出限0.06～0.08μg/L;高低两个水平的平均加标回收率分别为91.2%～102%和93.0%～99.0%;相对标准偏差(RSD)2.11%～3.264%;日内重复取样测定的RSD≤3.26%,日间重复取样测定的RSD≤4.36%。结论该方法可用于测定水中5种微囊藻毒素,方法操作简单、干扰少、快速、准确可靠,检测方法的检出限、精密度和加标回收率符合国家生活饮用水标准检验方法对质量控制的要求。

Determination of five microcystins in drinking water by HPLC/MS/MS

Objective A high performance liquid chromatography-tandem mass spectrometric method was established for determination of five microcystins(MC-LR,MC-LW,MC-RR,MC-LF,MC-YR)in drinking water and source water.Methods The five microcystins in water was cleaned by 0.22 μm millipore filter,then detected by high performance liquid chromatography-tandem mass spectrometry.Identification was achieved by electrospray ionization(ESI) in positive mode using multiple reaction monitoring.Results The calibration curves of five microcystins showed good linearity in the range of 0.5-50μg/L with correlation coefficient in the range of 0.9994-1.0000.The detection limit of the method was from 0.06μg/L to 0.08μg/L,the recoveries of two spiking levels ranged from 91.2% to 102%,and RSDs of range from 2.11% to 3.26% were obtained.Conclusion The method for determination of five microcystins in drinkingwater and source water by HPLC-MS/MS was of operation convenience,less interference from impurities and good accuracy,which could meet the requirements of national health standard method for the determination of microcystins in drinking water.