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[目的]构建一种固相萃取-液相色谱-串联质谱技术测定苹果中痕量吡虫啉残留量的方法。[方法]采用1%的醋酸-乙腈溶液为提取剂,以乙二胺-N-丙基硅烷(PSA)和硅胶(C18E)为分散净化剂的固相萃取方法提取苹果中的吡虫啉,并利用高效液相色谱-串联质谱法(HPLC-MS/MS)法进行检测。[结果]吡虫啉在0.005~1.0 mg/L之间呈良好的线性关系,线性相关系数为0.999 97;检出限(LOD)为0.0119 mg/kg;定量限(LOQ)为0.0397 mg/kg;在0.01、0.05、0.1 mg/kg三个添加水平上,苹果中吡虫啉的平均回收率在95%~100%之间,相对标准偏差(RSD)为2.2%~6.8%。[结论]方法操作简单、灵敏度高,满足现行法规要求,可实现苹果中吡虫啉的痕量测定。
[Objective] The research aimed to establish a method for the determination of trace imidacloprid residues in apples by solid phase extraction-liquid chromatography-tandem mass spectrometry. [Method] The imidacloprid in apple was extracted by solid-phase extraction with ethylenediamine-N-propylsilane (PSA) and silica gel (C18E) as dispersing agent with 1% acetic acid- High performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method. [Result] Imidacloprid had a good linear relationship in the range of 0.005-1.0 mg / L with a linear correlation coefficient of 0.999 97, a limit of detection (LOD) of 0.0119 mg / kg and a limit of quantitation (LOQ) of 0.0397 mg / kg. The average recoveries of imidacloprid in apples ranged from 95% to 100% and the relative standard deviations (RSDs) ranged from 2.2% to 6.8% at three levels of 0.01, 0.05 and 0.1 mg / kg. [Conclusion] The method was simple in operation and high in sensitivity, meeting the requirements of the current laws and regulations and enabling the trace determination of imidacloprid in apples.