液相色谱串联质谱法直接进样测定饮用水中的百草枯  

Direct sampling determination of paraquat in drinking water by liquid chromatography electrospray ionization tandem mass spectrometry

作　　者：郑和辉[1] 卞战强[1] 田向红[1] 于建[1] 查玉娥[1] 张娟[1] 

机构地区：[1]中国疾病预防控制中心农村改水技术指导中心,北京102200

出　　处：《中国卫生检验杂志》2014年第18期2602-2603,2608,共3页Chinese Journal of Health Laboratory Technology

基　　金：卫生行业科研专项(201302004)

摘　　要：目的建立利用液相色谱串联质谱通过直接进样测定水中百草枯的方法。方法水样过0.22μm滤膜,直接进液相色谱质谱分析,色谱柱:CAPCELL PAK ST柱(2.1 mm×150 mm)。结果百草枯在水中进行了4.0 ng/ml、10.0 ng/ml和40.0 ng/ml 3个水平的添加。通过测定和工作曲线的计算,得到的测定结果分别为(3.9±0.1)ng/ml,(10.7±0.2)ng/ml和(39.6±1.1)ng/ml,即平均回收率分别为97.5%、107.0%和99.0%。百草枯在水中浓度范围为1.0 ng/ml^40.0 ng/ml,它的线性相关系数为0.9992。在自来水中添加百草枯,以10倍信噪比(S/N)计算,在进样量10μl时,最低检测质量浓度0.05 ng/ml。结论该方法简单、速度快、准确度和灵敏度高,满足测定水中百草枯的需要。Objective To establish the method for direct sampling determination of paraquat in drinking water by liquid chromatography with tandem mass spectrometry. Methods Chromatographic column： CAPCELL PAK ST（ 2. 1 mm × 150 mm）; After passing 0. 22 μm filter membrane,samples were detected by LC- MS- MS. Results At three spiked level 4. 0 ng /ml,10. 0 ng /ml and 40. 0 ng /ml,the detected concentrations were（ 3. 9 ± 0. 1） ng /ml,（ 10. 7 ± 0. 2） ng /ml and（ 39. 6 ± 1. 1） ng /ml respectively. The average recoveries for paraquat in drinking water were 97. 5%,107. 0% and 99. 0%,respectively. The concentration of paraquat at 1. 0 ng /ml ~ 40. 0 ng /ml,its relativelinear coefficient value was 0. 9992. When the paraquat was added to the drinking water with 10 times signal- to- noise ration,the limit of detection（ S /N = 10） for paraquat was 0. 05 ng /ml.Conclusion The results showed that the method was simple and fast,and had a good accuracy and high sensitivity. So it can meet the need for determination of paraquat in drinking water.

关 键 词：百草枯 质谱 饮用水 

分 类 号：O657.633[理学—分析化学]