微波辅助净化-气相色谱法测定含硫蔬菜中有机磷农药残留

Determination of organophosphorus pesticide residues in sulfur-containing vegetables by gas chromatography with microwave-assisted clean-up treatment

中文关键词:  有机磷农药残留  微波辅助净化  基质分散固相萃取  含硫蔬菜  气相色谱法

英文关键词:organophosphorus pesticide residues  microwave-assisted clean-up treatment  matrix dispersive solid phase extraction  sulfur-containing vegetables  gas chromatography

中文摘要:

      目的 建立微波辅助净化-气相色谱法测定含硫蔬菜中有机磷农药残留的分析方法。方法 样品经微波预处理抑制酶促反应后, 使用乙腈提取、基质分散固相萃取净化、丙酮复溶、有机滤膜过滤后, 采用气相色谱-火焰光度检测器测定。结果 敌敌畏、甲胺磷、氧乐果、乐果、毒死蜱、水胺硫磷在0.01~0.50 μg/mL浓度范围内呈现良好的线性关系, 相关系数均大于0.999, 方法的检出限为0.0002~0.0004 mg/kg, 定量限为0.0008~0.0013 mg/kg; 有机磷农药在香葱、韭菜、白萝卜基质中加标0.002, 0.010, 0.100 mg/kg 浓度水平, 加标回收率为83.2%~104.7%, 相对标准偏差在2.3%~10.2% (n=6)。结论 本方法简便, 抗干扰能力强, 定量准确, 具有良好的重现性和稳定性, 能够有效的检测含硫蔬菜中有机磷农残的含量。

英文摘要:

      Objective To establish a method for determination of organophosphorus pesticide residues in sulfur-containing vegetables by gas chromatography with microwave-assisted clean-up treatment. Methods After microwave pretreatment of the sample to inhibit the enzymatic reaction, the sample was extracted with acetonitrile, purified by matrix-dispersed solid phase extraction, reconstituted with acetone, and filtered with an organic filter, and then determined by gas chromatography-flame photodetector. Results Dichlorvos, methamidophos, omethoate, dimethoate, chlorpyrifos, and amithion exhibited good linear relationship in the concentration range of 0.01? 0.50 μg/mL, the correlation coefficients were all greater than 0.999 mg/kg, and the limits of quantitation were 0.0008?0.0013 mg/kg. Organophosphorus pesticides spiked in chives, leeks, and white radish matrices at 0.002, 0.010, 0.100 mg/kg, the spiked recovery was 83.2%?104.7%, and the relative standard deviation was 2.3%?10.2% (n=6). Conclusion This method is simple, and has strong anti-interference ability, accurate quantification, good reproducibility and stability, which can effectively detect the content of organophosphorus pesticide residues in sulfur-containing vegetables.