冷冻诱导液液萃取结合超高效液相色谱-串联质谱法同时检测水果中12种烟碱类农药

Simultaneous determination of 12 kinds of nicotine pesticides in fruits by ultra performance liquid chromatography-tandem mass spectrometry coupled with cold induced liquid-liquid extraction

中文关键词:  液相色谱-串联质谱  水果  烟碱类农药

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  fruits  nicotine pesticides

中文摘要:

      目的 建立冷冻诱导液液萃取结合超高效液相色谱-串联质谱法同时检测水果中12种烟碱类农药的检测方法。方法 水果样品使用乙腈提取, 经盐析、振荡、离心后, 使用乙腈-水溶液进行冷冻诱导液液萃取, 进一步富集和净化, 结合超高效液相色谱质谱联用仪, 使用多反应监测模式采集数据, 同位素内标法定量。结果 12种烟碱类化合物在1~500 ng/mL线性范围内方法线性良好(r2＞0.999), 检出限为2.15~3.60 μg/kg, 方法定量限为7.11~13.01 μg/kg。12种烟碱类化合物加标回收率为73.1%~126.7%, 相对标准偏差为3.5%~13.3%。结论 该方法操作简便、精密度高、稳定性好, 适用于水果样品中烟碱类化合物的筛查检测工作。

英文摘要:

      Objective To establish a detection method for 12 kinds of nicotine pesticides in fruits by ultra performance liquid chromatography-tandem mass spectrometry coupled with cold induced liquid-liquid extraction. Methods Fruit samples were extracted using acetonitrile, and after salting out, shaking, and centrifugation, they were subjected to freeze induced liquid-liquid extraction using acetonitrile water solution for further enrichment and purification. Combined with ultra performance liquid chromatography mass spectrometry, data was collected using a multi reaction monitoring mode, and quantified using isotope internal standard method. Results The linear range of 12 kinds of nicotine compounds was 1–500 ng/mL, and the method showed good linearity (r2>0.999). The limits of detection were 2.15–3.60 μg/kg, and the method limits of quantification were 7.11–13.01 μg/kg. The recovery rates of 12 kinds of nicotine compounds were 73.1%–126.7%, and the relative standard deviations were 3.5%–13.3%. Conclusion This method is easy to operate, has high precision, and good stability, and is suitable for screening and detecting nicotine like compounds in fruit samples.