水中微囊藻毒素的超高效液相色谱-四极杆-静电场轨道阱高分辨质谱测定法  

Determination of microcystins in water by ultra high performance liquid chromatographyquadrupole-Orbitrap mass spectrometry

作　　者：周倩如[1] 何岸檐 杨伟[1] 张洁[1] 王正虹[1] 陈静[1] ZHOU Qian-ru;HE An-yan;YANG Wei;ZHANG Jie;WANG Zheng-hong;CHEN Jing(Institute for Physical and Chemical A nalyis and Toxicology Testing,Chongqing Center for Disease Control and Prevention,Chongqing 400042,China)

机构地区：[1]重庆市疾病预防控制中心理化与卫生毒理检测所,重庆400042

出　　处：《环境与健康杂志》2018年第6期524-527,共4页Journal of Environment and Health

基　　金：重庆市卫生计生委科技项目(2008-2-297)

摘　　要：目的建立水中微囊藻毒素(MC)煮沸浓缩-超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLCquadrupole-Orbitrap MS)的测定方法。方法水样在电热板上加热浓缩后,以0.22μm滤膜过滤,采用BEH C_(18)色谱柱(50mm×2.0 mm,2.1μm),以甲醇-2‰甲酸水溶液作为流动相,梯度洗脱,采用电喷雾电离源正离子模式(HESI+)在t-SIM模式下分析检测,通过测得的精确质量数与理论精确质量数吻合度、目标化合物的元素组成、保留时间进行定性。结果MC-LR、MC-YR、MC-RR、MC-LA、MC-LF、MC-LY在0.2～5μg/L,MC-WR在1～25μg/L之间线性良好,相关系数均>0.998;MC-RR、MC-YR、MC-LR、MC-WR、MC-LA、MC-LY、MC-LF的检出限分别为0.18、0.26、0.40、1.31、0.29、0.29、0.29ng/L;高、中、低浓度加标的RSD为4.11%～10.8%,平均回收率为61.8%～103%。结论该方法简便快捷,选择性好,灵敏度高,重现性好,可满足水中微囊藻毒素检测的要求。Objective To establish a method for the determination of microcystins in water using ultra high performance liquid chromatography-quadrupole-Orbitrap mass spectrometry. Methods Samples were heated and concentrated on electric heating plate,then filtered through 0.22 μm filter membrane. Sample purification was performed on BEH C18 column（50 mm×2.0 mm,2.1 μm） with the gradient elution of methanol and 2‰ formic acid. The samples were analyzed by using the electrospray ionization positive ion source（HESI+） and were scanned in the t-SIM mode,the objective compounds were qualitatively detected through the element compositions of target fragment,retention time and the matching level of accurate mass number and theoretical accurate mass number. Results The calibration curves showed great linearity between 0.2-5 μg/L for MC-LR、MCYR、MC-RR、MC-LA、MC-LF、MC-LY,between 1-25 μg/L for MC-WR,the correlation coefficient of them were all above 0.998. The method detection limits of MC-RR, MC-YR, MC-LR, MC-WR, MC-LA, MC-LY and MC-LF were 0.18, 0.26,0.40, 1.31, 0.29, 0.29 and 0.29 ng/L respectively. The average recoveries at three levels（low,moderate and high concentration）for each species were in the range of 61.8%-103%,the relative standard deviations were in the range of 4.11%-10.8%.Conclusion This method is easy to operate and shows high sensitivity,good selectivity and reproducibility,meets all the detection requirements of microcystins in water.

关 键 词：超高效液相色谱-四极杆-静电场轨道阱高分辨质谱 水 微囊藻毒素 

分 类 号：O657.6[理学—分析化学]