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目的建立一种同时测定蔬菜中49种农药残留量的固相萃取气相色谱-三重四极杆质谱(GC-MS/MS)的方法。方法样品经乙腈提取,43℃水浴中旋转蒸发近干,固相萃取小柱净化,样品液氮吹浓缩后,用气相色谱GC-MS/MS法测定,外标法定量。结果 49种农药在36 min内完全分离,在0.01~10μg/ml范围内相关系数r2均在0.99以上,加标回收率在71.60%~109.3%之间,相对标准偏差均小于12%,定性检出限为0.001~0.006μg/ml。结论该方法操作简单,准确度和精密度高,适用于各种蔬菜中农药多残留量的检测和确证。
OBJECTIVE To establish a method for the simultaneous determination of 49 pesticide residues in vegetables by solid-phase extraction and gas chromatography-triple quadrupole mass spectrometry (GC-MS / MS). Methods The samples were extracted with acetonitrile, evaporated to near dryness in 43 ℃ water bath and purified by solid phase extraction cartridge. The sample was concentrated by liquid nitrogen and determined by gas chromatography-mass spectrometry (GC-MS / MS) and external standard method. Results 49 kinds of pesticides were completely separated within 36 min. The correlation coefficients r2 were over 0.99 in the range of 0.01 ~ 10 μg / ml with recoveries of 71.60% -109.3%. The relative standard deviations were both less than 12% The limit is 0.001 to 0.006 μg / ml. Conclusion The method is simple, accurate and precise. It is suitable for the detection and confirmation of pesticide residues in vegetables.