【作者】 刘红河； 刘桂华； 朱舟； 陈裕华；

【Author】 LIU Hong-he,LIU Gui-hua,ZHU Zhou,CHEN Yu-hua. (Shenzhen Center for Disease Control & Prevention,Shenzhen 518055,China)

【机构】 深圳市疾病预防控制中心；

【摘要】 [目的]建立液相色谱-串联质谱法测定饮用水和水源水中五种微囊藻毒素的方法,以完善现有国标《生活饮用水卫生标准检测方法》有关内容。[方法]采用直接进样方式,用高效液相色谱一串联质谱(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,线性相关系数在0.9994-1.0000之间,检出限在0.06-0.08μg/L之间;高低两个水平的平均加标回收率分别在91.2%-102%和93.0%-99.0%之间;相对标准偏差(RSD)均小于4.4%。[结论]该方法用于测定饮用水和水源水中五种微囊藻毒素具有操作简单、干扰少、快速、准确可靠等特点,符合国家卫生标准方法建立的相关要求。更多还原

【Abstract】 Objective A high performance liquid chromatography-tandem mass spectrometric method was established for determination of five microcystins in drinking water and source water.Method The five microcystins in water was cleaned by 0.22μm 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.Result The calibration curves of five microcystins showed good linearity in the range of 0.5-50μg/Lwith 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%to102%,and RSDs of 4.4%or less were obtained.Conclusion The method for determination of five microcystins in drinking water 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 and source water更多还原