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目的建立测定中草药类保健食品中有机磷农药残留的分散固相萃取-分散液液微萃取-气相色谱-质谱联用法。方法样品经含0.5%甲酸的乙腈超声提取,上清液经含无水硫酸镁、N-丙基乙二胺(PSA)、C18的分散固相萃取管(d-SPE)净化后,采用分散液液微萃取(DLLME)步骤,用氯仿萃取、浓缩目标化合物。结果在最优条件下,线性范围为0.05~1.00μg/ml,线性相关系数在0.999以上,检出限(LOD)为0.3~3.0μg/kg,29种有机磷农药的平均加标回收率在70.3%~107.5%之间,相对标准偏差均<10%。结论该方法具有简便快速、准确灵敏、萃取效率高等特点,可用于中草药类保健食品中有机磷农药残留的检测。
OBJECTIVE To establish a dispersive solid-phase extraction-dispersive liquid-liquid microextraction-gas chromatography-mass spectrometry method for the determination of organophosphorus pesticide residues in Chinese herbal health food. Methods The samples were extracted by acetonitrile containing 0.5% formic acid. The supernatant was purified by d-SPE with anhydrous magnesium sulfate, N-propyl ethylenediamine (PSA) and C18. Liquid-liquid microextraction (DLLME) step, extraction with chloroform, concentration of the target compound. Results Under the optimized conditions, the linear range was 0.05-1.00 μg / ml, the linear correlation coefficient was above 0.999, and the limit of detection (LOD) was 0.3-3.0 μg / kg. The average recoveries of 29 organophosphorus pesticides were in the range of 70.3% ~ 107.5%, relative standard deviation <10%. Conclusion The method is simple, rapid, accurate and sensitive and has high extraction efficiency. It can be used for the determination of organophosphorus pesticide residues in Chinese herbal medicine health food.