梁秀美, 张井, 林定鹏, 何如意, 谢拾冰, 廖琳慧, 王亮, 徐静, 张维一. 基于改良QuEChERS-气相色谱-串联质谱法测定禽蛋中53种农药残留[J]. 农药学学报, 2021, 23(5): 973-985. DOI: 10.16801/j.issn.1008-7303.2021.0122
    引用本文: 梁秀美, 张井, 林定鹏, 何如意, 谢拾冰, 廖琳慧, 王亮, 徐静, 张维一. 基于改良QuEChERS-气相色谱-串联质谱法测定禽蛋中53种农药残留[J]. 农药学学报, 2021, 23(5): 973-985. DOI: 10.16801/j.issn.1008-7303.2021.0122
    LIANG Xiumei, ZHANG Jing, LIN Dingpeng, HE Ruyi, XIE Shibing, LIAO Linhui, WANG Liang, XU Jing, ZHANG Weiyi. Determination of 53 pesticide residues in poultry eggs by modified QuEChERS coupled with gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(5): 973-985. DOI: 10.16801/j.issn.1008-7303.2021.0122
    Citation: LIANG Xiumei, ZHANG Jing, LIN Dingpeng, HE Ruyi, XIE Shibing, LIAO Linhui, WANG Liang, XU Jing, ZHANG Weiyi. Determination of 53 pesticide residues in poultry eggs by modified QuEChERS coupled with gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2021, 23(5): 973-985. DOI: 10.16801/j.issn.1008-7303.2021.0122

    基于改良QuEChERS-气相色谱-串联质谱法测定禽蛋中53种农药残留

    Determination of 53 pesticide residues in poultry eggs by modified QuEChERS coupled with gas chromatography-tandem mass spectrometry

    • 摘要: 基于改良QuEChERS前处理方法结合气相色谱-串联质谱 (GC-MS/MS),建立了禽蛋中53种农药残留的检测方法。样品用乙酸乙酯提取,经弗罗里硅土和硅藻土净化,用GC-MS/MS分析。采用HP-5MS柱进行分离,电子轰击离子源 (EI) 动态多反应监测模式 (dMRM) 检测,以空白基质匹配标准溶液外标法定量。结果表明:经方法验证,53种农药的仪器检出限 (LOD) 在0.000 25~0.005 mg/L之间,方法定量限 (LOQ) 在0.000 5~0.01 mg/kg之间,相关系数 (r)在0.996 7~1之间;在LOQ、2 LOQ和10 LOQ 3个添加水平下,53种农药在鸡蛋中的平均回收率在76%~104%之间,相对标准偏差在0.090%~14%之间 (n = 6)。该方法前处理快速、检测方法灵敏、准确,在禽蛋中有机氯和有机磷等农药多残留检测中具有较好的应用前景。

       

      Abstract: In this study, an analytical method for the determination of 53 pesticide residues in poultry eggs was established using modified QuEChERS sample preparation and gas chromatography-tandem mass spectrometry. The pesticide residues in samples were extracted by ethyl acetate, cleaned-up with florisil and diatomite, and analyzed by GC-MS/MS. HP-5MS column was used for the separation, and the electron bombardment ion source (EI) was employed using dynamic multiple reaction monitoring (dMRM) mode for the detection. The matrix matched external standard calibration curves were used for quantitative analysis. The results indicated that the instrument limit of detection (LOD) for 53 pesticides were 0.000 25-0.005 mg/L, and the limit of quantification (LOQ) were 0.000 5-0.01 mg/kg for the method. The correlation coefficient (r) of the calibration curves for the compounds were 0.996 7-1. The average recoveries of 53 pesticides in hen’s eggs at three spiked levels (LOQ, 2LOQ and 10LOQ) were 76%-104% (n = 6) with relative standard deviations (RSDs) of 0.090%-14%. The method was rapid, sensitive and accurate, and has a good application prospect in the detection of organochlorine and organophosphorus pesticide residues in various poultry eggs.

       

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