超高效液相色谱法测定呼和浩特市饮用水中的微囊藻毒素-LR  

Ultra-high performance liquid chromatography for determination of microcystins-LR in drinking water

作　　者：赵宏[1] 胡芬[1] 图雅[1] 王建绣[1] 

机构地区：[1]呼和浩特市疾病预防控制中心,呼和浩特市010070

出　　处：《中国卫生检验杂志》2013年第6期1413-1414,共2页Chinese Journal of Health Laboratory Technology

基　　金：内蒙古呼和浩特市科技局重大专项(2010-重-农社-23)

摘　　要：目的:采用超高效液相色谱法(UPLC)测定呼和浩特市12个自来水水厂的微囊藻毒素-LR。方法:取水样5 L,GF/C过滤,滤液过C18柱,依次用50 ml去离子水,50 ml 20%甲醇淋洗,50 ml 80%甲醇洗脱,氮气吹干,残渣溶于1 ml甲醇,过0.45 um滤膜进样。采用C18色谱柱,流动相为乙腈+水+三氟乙酸(38+62+0.01),流速0.2 ml/min,PDA检测器检测。结果:微囊藻毒素-LR在0.3μg/ml～2.0μg/ml范围内线性良好(r=0.9998),且峰形好,回收率为70%～85%,精密度RSD为1.0%～5.0%,检出限为0.05μg/ml。结论:本法定性准确、灵敏度高、回收率和重现性好,操作快速。Objective： To establish the ultra -high performance liquid chromatography （UPLC） for determination of microcystin -LR in drinking water from 12 water plants of Hohhot. Methods： Water samples was filtered through GF/C on C18 column, then eluted by 50 ml deionized water, 50 ml 20% methanol and 50 ml 80% methanol in turn, dried by nitrogen, then the residues was dissolved in 1 ml methanol, filtered through 0.45 um membrane for injection on C18 chromatography column, with acetonitrile ＋ water ＋ trifluoroacetic acid （38 ＋ 62 ＋ 0. 01 ） as mobile phase at flow rate of 0.2 ml/min, and detected by PDA. Results： Microcystin -LR showed good linearity in the range of 0.3 ug/ml - 2.0 ug/ml （ r = 0. 9998 ） with good peak shape. The recoveries ranged from 70% to 85%, the RSD was 1.0% -5.0% , the detection limit was 0.05 ug/ml. Conclusion： The method is accurate, high sensitive, reproducible and quick to operate.

关 键 词：饮用水 微囊藻毒素-LR 超高效液相色谱法 PDA 

分 类 号：O657.72[理学—分析化学]