关键词: 气相色谱-串联质谱法, 菊花, 农药残留, 不确定度

Abstract: In order to establish the determination method of 29 pesticide residues in chrysanthemum by gas chromatography-tandem mass spectrometry and its uncertainty evaluation, the content of 29 pesticide residues in chrysanthemum was determined by gas chromatography-tandem mass spectrometry with internal standard method, and the uncertainty generated in the detection process was analyzed and evaluated by establishing a mathematical model according to the evaluation criteria and expression of the measurement uncertainty. It includes three aspects: preparation of standard solution, fitting of standard curve and determination of test products. The results showed that the linearity of the 29 pesticides in chrysanthemum- DOI:10.3969/j.issn.1000-1565.2024.02.005气相色谱-串联质谱法测定菊花中29种农药残留量的不确定度评价赵志磊^1,2,3,孙鸣^1,2,刘冬冬^1,2,李迅^1,2,马力辉^1,2(1.河北大学 质量技术监督学院,河北省能源计量与安全检测技术重点实验室,河北 保定 071002;2.河北大学 计量仪器与系统国家地方联合工程研究中心,河北 保定 071002;3.河北大学 地理标志研究院,河北 保定 071002)摘 要:为建立菊花中29种农药残留的气相色谱-串联质谱测定方法及不确定度评价,采用气相色谱-串联质谱内标法测定菊花中29种农药残留的含量,并依据测量不确定度的相关评定标准与表示,通过建立数学模型,对检测过程中产生的不确定度进行分析与评价,包括标准溶液配制、标准曲线拟合、供试品测定3大方面.结果表明:菊花中29 种农药质量浓度在0.002~0.1 mg/L内线性关系良好,回归方程决定系数R²为0.997 36~0.999 82,定量限0.002 03~1.18 963 mg/L,检出限0.000 64~0.356 89 mg/L,添加回收实验中测定平均回收率为69.85%~93.26%,29种农药测量数值为0.04、0.06、0.1 mg/kg时,得到扩展不确定度为0.004 787~0.058 935 mg/kg.测量结果不确定度显示标准工作液的配制和标准曲线拟合是本实验测定方法不确定度的主要影响因素,该实验结果可以为测定菊花中农药残留量的方法及不确定度评价提供参考.关键词:气相色谱-串联质谱法;菊花;农药残留;不确定度中图分类号:TS207.3 文献标志码:A 文章编号:1000-1565(2024)02-0146-10Uncertainty evaluation of 29 pesticide residues in chrysanthemum by gas chromatography-tandem mass spectrometryZHAO Zhilei^1,2,3, SUN Ming^1,2, LIU Dongdong^1,2, LI Xun^1,2, MA Lihui^1,2(1.Hebei Key Laboratory of Energy Metering and Safety Testing Technology, College of Quality and Technical Supervision, Hebei University, Baoding 071002, China; 2. National & Local Joint Engineering Research Center of Metrology Instrument and System, Hebei University, Baoding 071002, China; 3.Institute of Geographical Indications,Hebei University, Baoding 071002, China )Abstract: In order to establish the determination method of 29 pesticide residues in chrysanthemum by gas chromatography-tandem mass spectrometry and its uncertainty evaluation, the content of 29 pesticide residues in chrysanthemum was determined by gas chromatography-tandem mass spectrometry with internal standard method, and the uncertainty generated in the detection process was analyzed and evaluated by establishing a mathematical model according to the evaluation criteria and expression of the measurement uncertainty. It includes three aspects: preparation of standard solution, fitting of standard curve and determination of test products. The results showed that the linearity of the 29 pesticides in chrysanthemum- 收稿日期:2022-12-25;修回日期:2023-06-06 基金项目:河北省重点研发计划项目(21344801D) 第一作者:赵志磊(1977—),男,河北大学教授,博士,主要从事食品药品质量检测技术研究,E-mail:15930721279@163.com 通信作者:马力辉(1967—),男,河北大学教授,博士,主要从事检测技术及产品创新研究.E-mail:malihui@aliyun.com第2期赵志磊等:气相色谱-串联质谱法测定菊花中29种农药残留量的不确定度评价were good in the range of 0.002~0.1 mg/L, and the coefficient of determination R² was between 0.997 36~0.999 82. The limits of quantitation were 0.002 03~1.189 63 mg/L, and the limits of detection were 0.000 64~0.356 89 mg/L. In addition, the average recoveries were between 69.85% and 93.26%, and the extended uncertainties were between 0.004 787~0.058 935 mg/kg for the measured values of 0.04, 0.06 and 0.1 mg/kg for the 29 pesticides. The uncertainty of measurement results showed that the preparation of standard working solutions and the fitting of standard curve were the main factors affecting the uncertainty of the measurement method in this experiment. The results could provide reference for determination of pesticide residues in chrysanthemum and uncertainty evaluation.

Key words: gas chromatography-tandem mass spectrometry, the chrysanthemum, pesticide residues, the uncertainty