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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。
Objective To establish a method for simultaneous determination of 5 microcystin (MC-LR, MC-LR, MC-LF, MC-YR) in drinking water by liquid chromatography- tandem mass spectrometry. Methods Direct injection method was used to determine microcystins in drinking water and drinking water by high performance liquid chromatography-tandem mass spectrometry (HPLC / MS / MS). Water samples were filtered through 0.22μm microporous membrane, and were detected by HPLC / MS / MS electrospray ionization cation (ESI +), multiple reaction monitoring (MRM) mode and external standard method. Results The linear range of the method was 0.5-50.0μg / L with the linear correlation coefficient of 0.9994-1.0000 and the detection limit of 0.06-0.08μg / L. The average recoveries of the two methods were 91.2% -102% and 93.0% respectively, ~ 99.0%; relative standard deviation (RSD) 2.11% ~ 3.264%; RSD≤3.26% measured by intraday repeated sampling and RSD≤4.36% by day repeated sampling. Conclusion The method can be used for the determination of five microcystins in water. The method has the advantages of simple operation, less interference, quickness, accuracy and reliability. The detection limits, the precision and the recoveries of the detection methods are in line with the national standards of drinking water quality test. Control requirements.