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目的:建立固相微萃取(SPME)结合气相色谱-火焰光度检测器(GC-FPD)同时测定饮用水中27种有机磷农药残留的方法。方法:实验中对影响SPME萃取效率的萃取头、搅拌速度、萃取时间、萃取温度等条件进行了优化。最终确定的SPME条件为:PDMS-DVB萃取头,搅拌速度1150 rpm,萃取时间45 m in,萃取温度60℃。结果:27种有机磷农药的峰面积与其质量浓度均有良好的线性关系,相关系数均大于0.990;最小检测量为4.3~87 ng/L;样品的加标回收率为76.4%~112.9%(相对标准偏差为1.5%~9.7%)。结论:该方法具有分析速度快、灵敏度高、重现性好、预处理简单等优点。
Objective: To establish a method for simultaneous determination of 27 organophosphorus pesticide residues in drinking water by solid-phase microextraction (SPME) combined with gas chromatography-flame photometric detector (GC-FPD). Methods: In this experiment, the conditions of extraction head, stirring speed, extraction time, extraction temperature and so on which affect the extraction efficiency of SPME were optimized. The final SPME conditions were: PDMS-DVB extraction head, stirring speed 1150 rpm, extraction time 45 min, extraction temperature 60 ℃. Results: The peak area of 27 kinds of organophosphorus pesticides had a good linear relationship with the mass concentration, the correlation coefficient was greater than 0.990, the minimum detectable amount was 4.3 ~ 87 ng / L, and the spiked recoveries were 76.4% ~ 112.9% The relative standard deviation was 1.5% ~ 9.7%). Conclusion: The method has the advantages of fast analysis, high sensitivity, good reproducibility and simple pretreatment.