分散液相微萃取联合气相色谱质谱检测水中11种有机磷农药和阿特拉津方法的建立

发布时间：2018-08-13 17:37

【摘要】：目的建立分散液相微萃取-气相色谱质谱测定水样中11种有机磷农药和阿特拉津的方法。方法分别对气相色谱条件、气相质谱条件进行优化,以提高萃取效率,优选条件建立方法后检测自来水和河水水样中有机磷农药。取10mL水样,将200μL二甲苯和800μL甲醇分别作为萃取剂和分散剂并混合后,注入水样中乳化分散,离心后取1μL上层有机相进样分析。气相色谱采用HP-5毛细管色谱柱(30m×0.25mm,0.25μm)程序升温分离,质谱采用EI离子源,选择离子监测模式定量。结果待测农药和阿特拉津在2.0~50ng/mL范围内线性良好。方法检出限为0.12~1.38ng/mL,测定精密度为5.57%~9.85%。将该方法应用于自来水和河水的测定,加标回收率为75.5%~107%。结论方法简单快速,萃取和浓缩同时进行,轻质萃取剂在萃取后更易取出,适用于水样中有机磷农药的分析。
[Abstract]:Objective to establish a method for the determination of 11 organophosphorus pesticides and atrazine in water samples by dispersive liquid phase microextraction-gas chromatography-mass spectrometry. Methods the conditions of gas chromatography and mass spectrometry were optimized to improve the extraction efficiency and to determine organophosphorus pesticides in tap water and river water samples after the establishment of optimal conditions. Taking 10mL water sample, 200 渭 L xylene and 800 渭 L methanol were mixed as extractant and dispersant respectively, then injected into water sample to emulsify and disperse. After centrifugation, 1 渭 L upper layer organic phase was analyzed. The HP-5 capillary column (30m 脳 0.25mm ~ 0.25 渭 m) was used to separate the gas by programmed temperature. The mass spectrometry was performed with ei ion source and the mode of ion monitoring was selected. Results the linear range of pesticide and atrazine was good in 2.0~50ng/mL range. The detection limit was 0.12 ~ 1.38 ng 路mL ~ (-1) and the precision was 5.57 ~ 9.85. The method has been applied to the determination of tap water and river water. Conclusion the method is simple and rapid, the extraction and concentration are carried out at the same time, and the light extraction agent is easier to be extracted after extraction, which is suitable for the analysis of organophosphorus pesticides in water samples.
【作者单位】：四川大学华西公共卫生学院卫生检验与检疫系食品安全检测与风险评估四川省重点实验室;
【分类号】：O657.63;R123

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