LC-MS/MS法测定赣江水中微囊藻毒素的初步研究  

The Preliminary Study on the Determination of Three Microcystins in the Ganjiang River by HPLC-MS/MS

作　　者：林芬[1] 邱伟[1] 刘艳红[1] 李舒梅[1] 刘大娇 程文炜 詹晓民 

机构地区：[1]赣南医学院预防医学系,江西赣州341000 [2]赣南医学院

出　　处：《赣南医学院学报》2016年第3期347-349,354,共4页JOURNAL OF GANNAN MEDICAL UNIVERSITY

基　　金：江西省教育厅科技项目;赣教技字[2006]254号;江西省教育厅科技项目(NO:GJJ11209);赣州市科技局课题;赣市科发[2005]20号;赣市财教字[2005]33号

摘　　要：目的:建立微囊藻毒素(MC-LR,MC-RR和MC-YR)的固相萃取-高效液相色谱串联质谱(LC-MS/MS)分析方法,测定赣江水中微囊藻毒素含量。方法:采集赣江水样18份,通过固相萃取柱富集净化,在电喷雾正离子模式下,以多反应监测模式采集数据,对微囊藻毒素进行定性与定量分析。结果:方法的线性范围为1.0~20μg·L^(^(-1)),线性相关系数0.999 8~0.999 9,检出限量为20 ng·L^(^(-1)),平均回收率为66%~88.73%;相对标准偏差(RSD)为4.11%~12.78%。18份水样中均未检出微囊藻毒素,达到《生活饮用水卫生标准》(GB5749-2006)。结论:该方法用来测定水中微囊藻毒素,操作快速简单、干扰少、准确;由于微囊藻毒素受采样时间、光照和气温等因素的影响,应持续监测水样,以保证赣江水质符合标准。Objective： A high performance liquid chromatography-tandem mass spectrometric was established for the determination of three microcystins（ MC-LR,MC-RR,MC-YR） in the Ganjiang River. Methods： Eighteen samples from the Ganjiang River were enriched and purified by solid phase extraction column,then detected by a high performance liquid chromatography-triple quadrupole mass spectrometer. The identification was achieved by electrospray ionization（ ESI） in positive mode using multiple reaction monitoring. Results： The calibration curves of three microcystins showed good linearity in the range of 1 ～ 20 μg·L（-1）,with correlation coefficient in the range of 0. 999 8 ～ 0. 999 99. The detection limit of the method was 20 ng·L（-1）. The recovery of two spiking levels ranged from 66% to 88. 73%,and RSDs ranged from4. 11% to 12. 78%. Microcystins were not detected in 18 samples of the Ganjiang River,showing that the water quality reached ＂ Sanitary Standards for Drinking Water＂. Conclusion： The method for the determination of microcystins of the Ganjiang River by HPLC-MS/MS was of operation convenience,less interference from impurities and good accuracy. The levels of Microcystins were influenced by sampling time,illumination,and temperature. Therefore,microcystins should be monitored in order to ensure the water quality of the Ganjiang River.

关 键 词：LC-MS/MS 微囊藻毒素 赣江 

分 类 号：R123.1[医药卫生—环境卫生学]