余巍, 桂英爱, 毛希琴, 李海燕, 张敬波. 气相色谱-串联质谱法测定葡萄中78种农药残留的定量校准方法评估[J]. 农药学学报, 2022, 24(1): 189-196. DOI: 10.16801/j.issn.1008-7303.2021.0136
    引用本文: 余巍, 桂英爱, 毛希琴, 李海燕, 张敬波. 气相色谱-串联质谱法测定葡萄中78种农药残留的定量校准方法评估[J]. 农药学学报, 2022, 24(1): 189-196. DOI: 10.16801/j.issn.1008-7303.2021.0136
    YU Wei, GUI Ying’ai, MAO Xiqin, LI Haiyan, ZHANG Jingbo. Evaluation of the calibration method on quantification of 78 pesticides in grape by gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(1): 189-196. DOI: 10.16801/j.issn.1008-7303.2021.0136
    Citation: YU Wei, GUI Ying’ai, MAO Xiqin, LI Haiyan, ZHANG Jingbo. Evaluation of the calibration method on quantification of 78 pesticides in grape by gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2022, 24(1): 189-196. DOI: 10.16801/j.issn.1008-7303.2021.0136

    气相色谱-串联质谱法测定葡萄中78种农药残留的定量校准方法评估

    Evaluation of the calibration method on quantification of 78 pesticides in grape by gas chromatography-tandem mass spectrometry

    • 摘要: 以柠檬酸盐缓冲体系的QuEChERS方法为前处理方法,气相色谱-串联质谱联用仪为检测仪器,建立了葡萄中78种农药残留的检测方法。采用添加回收法评估了葡萄中4种基质匹配校准方法的定量结果,评估了4种校准方法的线性回归系数、回收率和精密度。结果表明:在添加回收试验中,当添加水平为0.01 mg/kg时,在0.005~0.1 mg/L范围内,4种校准方法下78种农药的质量浓度与对应的峰面积间线性关系良好,R2均大于0.99,大部分农药的精密度均可满足农药残留检测的要求。在使用以空白基质溶液配制的标准工作溶液进行校准时,无论是外标法还是内标法,回收率均无法兼顾所有分析对象;而改用基质匹配标准溶液得到的基质标准曲线表现更好,其外标法和内标法的回收率范围分别为82%~114%和81%~110%,相对标准偏差范围分别为2.3%~18%和1.2%~17%,符合食品理化检测的质量控制要求,适合实验室日常监测采用。

       

      Abstract: A method was established for the simultaneous determination of 78 pesticides in grapes by QuEChERS sample preparation with a citrate buffer and gas chromatography-tandem mass spectrometry (GC-MS/MS). The quantitative results of four matrix matching calibration methods in grapes were evaluated by spiking recovery method, and the linear regression coefficient, recovery, and precision of the four calibration methods were evaluated. The results showed that when the spiking level was 0.01 mg/kg, the linear relationships between peak area and mass concentration of 78 pesticides using the four calibration methods in the range of 0.005-0.1 mg/L were good and the determination cofficients (R2) were all above 0.99, and the precision of most pesticides could meet the requirements of pesticide residue detection. However, when the matrix matched calibration that prepared with blank matrix extracts was used for calibration, whether with internal standard or not, the recoveries were not satisfactory for all the compounds. Much better recovery results were obtained using the matrix matched calibration that prepared by blank matrix spiked with standard solutions, with or without internal standard, the recoveries were in the range of 82%-114% and 81%-110%, respectively, and the relative standard deviations were 2.3%-18% and 1.2%-17%, respectively. The method meets the quality control criterion on chemical testing of foods, and is suitable for routine analysis in laboratory.

       

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