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Validation of a modified QuEChERS method to determine multiclass multipesticide residues in apple, banana and guava using GC–MS and LC–MS/MS and its application in real sample analysis

机译:使用GC-MS和LC-MS / MS验证改良的QuEChERS方法以确定苹果,香蕉和番石榴中多种农药残留的方法及其在实际样品分析中的应用

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A modified QuEChERS method was developed for the determination of 64 pesticides in apple, guava andbanana usingGC–MS and LC–MS/MS. Out of sixty-four pesticides, 39 (32 insecticides + 7 herbicides) were analysed by GC–MS and otherswere analysed in LC–MS/MS. The efficiency of methanol, ethyl-acetate and acetonitrile as extracting solvents werechecked. Among these, acetonitrile gave the highest recovery. D-SPE clean-up was done for apple and guava using PSA,whereas PSA + GCB was used for banana to remove heteropolysaccharides and carotenoids. The method was validatedas per SANTE/11813/2017 guidelines. The LOD was in the range of 0.002–0.04 mg kg~(−1) and LOQ was 0.005–0.11 mg kg~(−1).Average recovery ranged from 80 to 120% with RSD ≤ 20% and RPD % of precision ≤ 20%. The expanded uncertaintywas ≤ 20%. The validated method was applied to check the real samples of apple, guava and banana collected frommarkets of four different districts of West Bengal, India.
机译:开发了一种改良的QuEChERS方法,用于测定苹果,番石榴和香蕉中的64种农药GC–MS和LC–MS / MS。通过GC-MS分析了64种农药中的39种(32种杀虫剂+ 7种除草剂)。在LC–MS / MS中进行了分析。甲醇,乙酸乙酯和乙腈作为萃取溶剂的效率为检查。其中,乙腈的回收率最高。使用PSA对苹果和番石榴进行了D-SPE净化,而PSA + GCB用于香蕉去除杂多糖和类胡萝卜素。该方法已经过验证根据SANTE / 11813/2017指南。 LOD在0.002-0.04 mg kg〜(-1)范围内,LOQ在0.005-0.11 mg kg〜(-1)范围内。RSD≤20%,RPD%精度≤20%时,平均回收率介于80%至120%之间。扩大的不确定性≤20%。经验证的方法用于检查从苹果中收集的苹果,番石榴和香蕉的真实样品印度西孟加拉邦四个不同地区的市场。

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