固相萃取-超高效液相色谱三重四级杆质谱联用法测定水中微囊藻毒素  

Determination of three microcystins in water by ultra performance liquid chromatography combined with MS

作　　者：顾海东[1] 尹燕敏[1] 秦宏兵[1] 

机构地区：[1]苏州市环境监测中心站,江苏苏州215004

出　　处：《苏州科技学院学报（工程技术版）》2012年第4期1-4,共4页Journal of Suzhou University of Science and Technology （Engineering and Technology）

基　　金：水体污染控制与治理科技重大专项(2009ZX07313-007)

摘　　要：建立了同时测定水样中3种微囊藻毒素MC—RR、MC—LR、MC—YR的固相萃取一超高效液相色谱三重四级杆质谱的方法。水样采用HLB固相萃取小柱富集和净化，甲醇溶液洗脱，过0．20μm滤膜后，利用超高效液相色谱三重四级杆质谱检测。在该方法的试验条件下，MC-RR、MC-LR、MC-YR的线性范围在1．0～200．0μ/L之间，3．143倍信噪比下最低检出限分别为2．6ng／L（MC-RR）、2．7ng／L（MC-YR、MC—LR）。方法用于分析实际水样，平均加标回收率分别为95．2％～10014％之间，相对标准偏差（n=7）在3．0％～8．7％之间。This paper presented the simultaneous determination of Microcystins （MC-RR, MC-YR, MC-LR） in water samples by ultra performance liquid chromatograph （UPLC） with solid phase extraction （SPE）. The water sample was purified and enriched by HLB column, microcystins were extracted with methanol and quantified with electrospray ionization mass spectrometry process （ESI-MS/MS）. The determination limits of the method were 2.6 and 2.7 ng/L for MC-RR and MC-YR, MC-LR, and linear arranges were 1.0-200.0 g/L for microcystins. Recov eries of microcystins ranged from 95.2% to 100. 4%. The RSD of determination ranged from 3.0% to 8.7%. The method offered traits of high sensitivity, speediness and exactness, and was applied to the determination of MC- RR and MC-LR in water samples with satisfactory results.

关 键 词：超高效液相色谱 三重四级杆质谱 微囊藻毒素 

分 类 号：O657.63[理学—分析化学]