全自动固相萃取-高效液相色谱法同时测定饮用水中2种微囊藻毒素和西维因  

Simultaneous determination of 2 microcystins and carbaryl in drinking water by automated solid phase extraction-high performance liquid chromatography

作　　者：方晓丽 李瑞芬[1] 张秀尧[1] 张晓艺[1] 郑三燕[1] 杨舒然 FANG Xiao-li;LI Rui-fen;ZHANH Xiu-yao;ZHANG Xiao-yi;ZHENG San-yan;YANG Shu-ran(Wenzhou Municipal Center for Disease Control and Prevention,Wenzhou,Zhejiang 325000,China)

机构地区：[1]温州市疾病预防控制中心,浙江温州325000

出　　处：《中国卫生检验杂志》2022年第13期1564-1566,1570,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立全自动固相萃取高效液相色谱同时测定饮用水中2种微囊藻毒素和西维因的方法。方法水样经全自动固相萃取仪净化富集,洗脱液经氮吹近干后用0.1%三氟乙酸甲醇定容,过0.45μm聚醚砜滤膜,滤液上液相色谱检测。实验采用XBridgeBEH(4.6 mm×75 mm,2.5μm)色谱柱分离,以乙腈和0.1%三氟乙酸溶液为流动相进行梯度洗脱,二极管阵列检测器检测。结果在0.20 mg/L~5.00 mg/L质量浓度内具有良好的线性关系(r>0.9999),方法检出限为0.03μg/L~0.04μg/L,定量限为0.1μg/L~0.2μg/L。3种分析物的加标回收率为76.9%~106.0%,相对标准偏差(RSD)为3.2%~6.4%(n=6)。结论该方法简便、准确、富集倍数高,适用于饮用水中2种微囊藻毒素和西维因的同时检测。Objective A method was developed for the simultaneous determination of 2 microcystins and carbaryl in drinking water by automated solid phase extraction-high performance liquid chromatography( HPLC). Methods The water sample was purified and enriched by automated solid phase extraction. The eluents were nearly dried up by a gentle stream of nitrogen. The residues were dissolved by methanol containing 0. 1%( V/V) trifluoroacetic and then filtered through 0. 45 μm polyether sulfone( PES) syringe filter. The filtrates were injected into HPLC system. The separation of the analytes was carried out on a XBridgeBEH column(4. 6 mm × 75 mm,2. 5 μm) with gradient elution mode using a mobile phase made of acetonitrile and 0. 1%( V/V) trifluoroacetic aqueous solution. The analytes were detected by diode array detector. Results In the range of 0. 20 mg/L-5. 00 mg/L,three analytes showed good linearity with the correlation coefficients( r) larger than 0. 999 9. The limits of detection were in the range of 0. 03 μg/L-0. 04 μg/L and the limits of quantification were within 0. 1 μg/L-0. 2 μg/L. The recoveries in spiked samples were in the range of 76. 9%-106. 0% and the relative standard deviations( RSDs) were in the range of 3. 2%-6. 4%( n = 6). Conclusion The method is simple,accurate and high concentrated. It can be applied to the simultaneous detection of 2 microcystins and carbaryl in drinking water.

关 键 词：高效液相色谱 全自动固相萃取 微囊藻毒素 西维因 饮用水 

分 类 号：O657.72[理学—分析化学]