摘要
目的建立液相色谱-串联质谱联用法母离子扫描模式快速筛查水质中有机磷农药的方法。方法以常见的116种有机磷农药为研究对象,依据化合物的结构和质谱裂解特点将其分类,筛选共有的子离子碎片,优化质谱参数,建立了母离子扫描模式的液质筛查方法。考察方法的专一性、线性、灵敏度、精密度和加标回收,并应用于实际样品的测定。结果方法专一性好,灵敏度高,水中116种目标化合物的检出限均低于20 ng/ml;在浓度为50 ng/ml^5 000 ng/ml时,线性关系良好,相关系数(r)均>0.98;3种添加水平的加标回收率为78.5%~112.1%;相对标准偏差为3.4%~23.2%。结论该方法测定速度快、灵敏高、专一性好,适合水质中有机磷农药污染的快速筛查,同时,还可以筛查新的有机磷农药品种。
Objective To develop the method for screening organophosphorus pesticides in water with liquid chromatography tandem mass spectrometry（ LC- MS） in parent ion scanning mode. Methods 116 organophosphorus pesticides were collected as the experimental examples,which were classified according to the structure and mass spectrum characteristics of the compounds,and their common ion fragments were screened. Then high performance liquid chromatography- tandem mass spectrometry（ HPLC- MS/MS） method in parent ion scanning mode was established based on the optimization of MS parameters. Linearity,sensitivity,specificity and precision and recovery were studied. The method was applied to determine actual samples. Results The developed method was proved to be specific and sensitive,with the limit of detection（ LOD） values for 116 organophosphorus pesticides all under 20 ng/ml in water; good linearity was obtained when the concentration was within 50 ng/ml-5 000 ng/ml,with the correlation coefficient（ r） greater than 0. 98; the spiked recoveries at three levels was within 78. 5%-112. 1%,with relative standard deviation（ RSD） within 3. 4%- 23. 2%. Conclusion The method shows advantages in sensitivity,specificity and efficiency,and is suitable for rapid screening of existing organophosphorus pesticides and unknown organophosphorus pesticides in water.
作者
李帮锐
冯家力
曾栋
丁力
刘先军
张昊
LI Bang - rui FENG Jia - li ZENG Dong DING Li LIU Xian - jun ZHANG Hao(Hunan Provincial Center for Disease Control and Prevention, Changsha, Hunan 410005, China)
出处
《中国卫生检验杂志》
CAS
2016年第20期2889-2893,2905,共6页
Chinese Journal of Health Laboratory Technology
基金
国家卫生部卫生标准制定项目(20130106)
关键词
液相色谱-串联质谱
母离子扫描
有机磷农药
水质
Liquid chromatography-tandem spectrometry
Parent ion scanning
Organophosphorus pesticides
Water quality
