分散液液微萃取-超高效液相色谱-串联质谱法测定市售凉茶中6种有机磷农药残留

Determination of 6 kinds of organophosphorus pesticide residues in commercial herbal tea by dispersive liquid-liquid microextraction-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  分散液液微萃取  超高效液相色谱-串联质谱  有机磷  凉茶

英文关键词:dispersive liquid-liquid microextraction  ultra performance liquid chromatography-tandem mass spectrometry  organophosphorus pesticide  herbal tea

中文摘要:

      目的 建立分散液液微萃取-超高效液相色谱-串联质谱法测定凉茶中6种有机磷残留量的方法。 方法 样品经N-丙基乙二胺(N-Propylethylenediamine, PSA)固相萃取剂预净化后, 以甲醇为分散剂, 三氯甲烷为萃取剂进行提取。在优化后的仪器条件下, 采用电喷雾离子化正离子模式电离, 多反应监测模式进行测定。结果 6种有机磷的标准曲线在2.0~200 μg/L范围内线性良好, 相关系数r2均大于0.9990, 在添加水平为0.25、0.50和2.5 μg/kg的加标回收试验中, 平均回收率范围为73.6%~99.5%, 相对标准偏差为1.14%~8.01%, 方法检出限和定量限为0.02~0.04 μg/kg和0.06~0.10 μg/kg。结论 该方法操作简单便捷、富集倍数高、灵敏度高、重现性好, 可用于实际市售凉茶产品的质量监督。

英文摘要:

      Objective To establish a method for the determination of 6 kinds of organophosphorus pesticide residues in commercial herbal tea by dispersive liquid-liquid microextraction-ultra performance liquid chromatography-tandem mass spectrometry. Methods Sample was pre-purified by N-propylethylenediamine (PSA) solid phase extractant, then extracted by methanol and chloroform which used as dispersant and extractant respectively, finally ionized by electrospray ionization positive ion mode and detected by multi-selected reaction monitoring under optimized instrument conditions. Results The calibration curves of 6 organophosphorus pesticide exhibited a good linearity in the range of 2.0–200 μg/L, all correlation coefficients were greater than 0.9990. In the spiked recovery test with addition levels of 0.25, 0.50 and 2.5 μg/kg, the average recoveries were 73.6%–99.5%, while the relative standard deviations were 1.14%–8.01%. The limits of detection and limits of quantitation were 0.02–0.04 μg/kg and 0.06–0.10 μg/kg, respectively. Conclusion This method is simple and convenient to operate, has high enrichment multiples, high sensitivity, and good reproducibility, and can be used for the quality supervision of actual commercially available herbal tea products.