固相萃取-高效液相色谱法同时检测生活饮用水中的呋喃丹、莠去津、微囊藻毒素-LR  

Simultaneous determination of Carbofuran,Astrazine and Microcystin-LR in drinking water by SPE-HPLC

作　　者：胡晓科[1] 冯波[1] 杨晓松[1] 

机构地区：[1]成都市疾病预防控制中心,四川成都610041

出　　处：《中国卫生检验杂志》2015年第11期1699-1702,共4页Chinese Journal of Health Laboratory Technology

基　　金：四川省科技支撑计划项目(2012SZ0196)

摘　　要：目的建立同时检测饮用水中的呋喃丹、莠去津、微囊藻毒素-LR的高效液相色谱分析方法。方法用C18固相萃取小柱同时富集水中痕量的呋喃丹、莠去津、微囊藻毒素-LR,经15%甲醇溶液净化后,用含1%甲酸的甲醇洗脱。样品通过高效液相色谱仪进行分析,以甲醇-水(0.05%甲酸)为流动相作梯度洗脱,在Agilent ZORBAX Eclipse XDBC18柱上进行分离,检测波长为238 nm。结果该方法测定呋喃丹的线性范围为0.00μg/ml^50.00μg/ml、莠去津为0.00μg/ml^10.00μg/ml、微囊藻毒素-LR为0.00μg/ml^5.00μg/ml,相关系数均>0.999;3种物质在0.000 6 mg/L^0.018 0 mg/L的加标回收率为80.6%~102.0%,RSD均<5.4%;呋喃丹、莠去津、微囊藻毒素-LR的最低检测浓度分别为0.4μg/L、0.05μg/L、0.2μg/L。结论该方法可同时检测生活饮用水中3种新指标,与国家标准分析方法相比,过程更加简化,检测结果准确、灵敏、可靠。Objective To establish the high - performance chromatographic method for simultaneous determination of Carbofu- ran, Astrazine and Microcystin - LR in drinking water. Methods Trace amounts of Carbofuran, Astrazine and Microcystin - LR were concentrated by Cls SPE cartridges, and eluted by methanol （ 1.0% HCOOH） after leaching with 15% methanol aque- ous solution. Samples were detected by a high - performance chromatographic system. The chromatographic separation was a- chieved on Agilent ZORBAX Eclipse XDB - Cls column with gradient elution by methanol/water （0.05% HCOOH）. The solute detection was made at 238 nm. Results The Linearity range was among 0. 00 μg/ml - 50.00 μg/ml for Carbofuran, 0. 00 μg/ml - 10.00 μg/ml for Astrazine, and 0.00μg/ml - 5.00 μg/ml for Microcystin - LR. The correlation coefficients were greater than 0. 999. The recoveries were from 80.6% to 102.0% within the range of 0.000 6mg/L -0. 018 0mg/L, RSD was less than 5.4%. The detection limit of the above target compounds was 0. 4 μg/L, 0.05 μg/L and 0.2 μg/L, respective- ly. Conclusion Using this method, three monitoring objects in drinking water can be determined simultaneously. In comparison to the standard analytic method, this new method is simpler, more accurate and more reliable.

关 键 词：饮用水 固相萃取-高效液相色谱法 呋喃丹 莠去津 微囊藻毒素 

分 类 号：O657.72[理学—分析化学]