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目的建立高效液相色谱-串联质谱法同时测定中草药保健食品中15种有机磷和氨基甲酸酯类农药残留。方法样品经乙腈提取后,高速离心,经分散型固相萃取小柱净化。采用Atlantis C_(18)(2.1 mm×100 mm,3μm)柱,以0.1%甲酸-乙腈为流动相,梯度洗脱分离。质谱采用正离子模式(electrospray ionization,ESI+),多反应监测模式(multiple reaction monitoring,MRM)进行检测,基质曲线外标法定量。结果该方法对15种农药残留的线性范围为0.001~0.1μg/mL,线性相关系数r≥0.993,加标回收率为82.7%~113.3%,相对标准偏差为2.7%~10.6%,检出限为0.8~24.6μg/kg。结论本方法操作简单、快捷,适用于中草药保健食品中15种有机磷和氨基甲酸酯类农药残留的同时检测,为保健食品质量控制提供依据。
OBJECTIVE To establish a method for simultaneous determination of 15 organophosphorus and carbamate pesticide residues in Chinese herbal health food by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile, centrifuged at high speed and purified by dispersive SPE column. Atlantis C_ (18) (2.1 mm × 100 mm, 3 μm) column was used with 0.1% formic acid-acetonitrile as the mobile phase and separated by gradient elution. Mass spectra were detected by electrospray ionization (ESI +), multiple reaction monitoring (MRM), and quantified by external standard curve. Results The linear range of this method was 0.001 ~ 0.1 μg / mL for 15 kinds of pesticide residues. The linear correlation coefficient was 0.993. The recoveries were 82.7% ~ 113.3%. The relative standard deviations were 2.7% ~ 10.6%. The detection limits 0.8 ~ 24.6μg / kg. Conclusion The method is simple, rapid and suitable for the simultaneous detection of 15 kinds of organophosphorus and carbamate pesticide residues in health food of Chinese herbal medicine, providing the basis for the quality control of health food.