超高效液相色谱-串联质谱法快速检测自来水中的12种微囊藻毒素  

Rapid determination of 12 microcystins in tap water by ultra-performance liquid chromatography tandem mass spectrometry

作　　者：王军淋[1] 韩见龙[1] 张念华[1] 冯靓[1] 张晶[1] 蔡增轩[1] WANG Jun-lin;HAN Jian-long;ZHANG Nian-hua;FENG Liang;ZHANG Jing;CAI Zeng-xuan(Zhejiang Provincial Center for Disease Control and Prevention,Hangzhou,Zhejiang 310051,China)

机构地区：[1]浙江省疾病预防控制中心,浙江杭州310051

出　　处：《中国卫生检验杂志》2022年第15期1801-1806,1810,共7页Chinese Journal of Health Laboratory Technology

基　　金：浙江省卫生和计划生育委员会青年人才项目(201827-0577)。

摘　　要：目的 建立自来水中12种微囊藻毒素(MCs)的超高效液相色谱-串联质谱快速检测法。方法 水样采集时,按80 mg/L加入硫代硫酸钠消除余氯对MCs的破坏,经玻璃纤维滤膜过滤后,直接进样分析。若MC低于定量限,则采用HLB柱富集,甲醇洗脱后加入等比例纯水稀释,经玻璃纤维滤膜过滤后进样分析。以0.2%甲酸水溶液和0.2%甲酸甲醇-乙腈溶液(40+60,体积比)作为流动相进行梯度洗脱,采用ACQUITY UPLC BEH C_(18)柱(100 mm×2.1 mm,1.7μm)分离,电喷雾正离子扫描模式下多反应监测方式检测,外标法定量。结果 12种MCs浓度在0.10 ng/ml~5.00 ng/ml时,线性相关系数(r)> 0.995,方法检出限为0.006μg/L~0.012μg/L(SPE法)、0.03μg/L~0.06μg/L(直接进样法)回收率为80.76%~110.68%,相对标准偏差为0.84%~5.88%(n=6)。结论 该方法简单、灵敏、准确,适用于自来水中12种MCs的快速检测。Objective A rapid method was established for rapid determination of 12 microcystins( MCs) in tap water by ultra-performance liquid chromatography tandem triple quadrupole mass spectrometry(UPLC-MS/MS).Methods When water samples were collected,sodium thiosulfate was added at 80 mg/L to eliminate the damage caused by residual chlorine to MCs.After filtration by glass fiber membrane,samples were directly injected for analysis.If MC is lower than the limit of quantification,it is enriched by HLB column,diluted with equal proportion of pure water after methanol elution,and filtered by glass fiber membrane before sampling analysis.Gradient elution was performed with 0.2% formic acid aqueous solution and 0.2%formic acid methanol-acetonitrile solution(40 + 60,V/V) as mobile phases.Separation was performed on ACQUITY UPLC BEH C_(18)column(100 mm × 2.1 mm,1.7 μm).Multiple reaction monitoring was performed in positive electrospray ionization(ESI) scanning mode.External standard method was adopted for quantification.Results The linear correlation coefficient(r)was greater than 0.995 when the concentration of 12 kinds of MCs ranged from 0.10 ng/ml to 5.00 ng/ml.The detection limits were within 0.006 μg/L-0.012 μg/L(SPE method) and 0.03 μg/L-0.06 μg/L(direct injection method).The recoveries were within 80.76%-110.68% with relative standard deviations of 0.84%-5.88%(n= 6).Conclusion The method is rapid,simple,sensitive and accurate,and can be applied for the determination of 12 microcystins in tap water.

关 键 词：超高效液相色谱-串联质谱法 微囊藻毒素 固相萃取 自来水 

分 类 号：O657.63[理学—分析化学]