1. Tangshan Food and Drug Comprehensive Testing Center, Tangshan, Hebei 063000, China
2. Hebei Agricultural Products Quality and Safety Testing Innovation Center, Tangshan, Hebei 063000, China
3. Tangshan Institute of Industrial Technology for Functional Agricultural Products, Tangshan, Hebei 063000,China
Abstract：According to NY/T 761—2008, the uncertainty of HCH, pythium, bifenthrin, beta cypermethrin, permethrin and cypermethrin in vegetables were evaluated by gas chromatography. The uncertainty of the detection method was evaluated from seven aspects: standard purity, standard solution, sample weighing, pretreatment process, standard solution peak, sample solution peak and recovery. The results showed that: at the spiking level of 0.08mg/kg, the relative combined standard uncertainty of α-HCH, β-HCH, γ-HCH, δ-HCH, Pythium, bifenthrin, beta Cypermethrin, permethrin and cypermethrin were 2.63%, 3.01%, 2.45%, 2.69%, 2.33%, 1.83%, 2.41%, 3.34% and 2.84%, respectively. The main factors of uncertainty were recovery, sample solution peak and standard solution peak. Standard solution and pretreatment process can not be ignored especially for the target with less measurement uncertainty.
张丽芳,张亮,杜瑞焕,郑百芹,刘洋. 气相色谱法测定蔬菜中农药残留量的测量不确定度评定[J]. 计量学报, 2022, 43(7): 965-972.
ZHANG Li-fang,ZHANG Liang,DU Rui-huan,ZHENG Bai-qin,LIU Yang. Evaluation of Measurement Uncertainty in the Determination of Pesticides Residues in Vegetables by Gas Chromatography. Acta Metrologica Sinica, 2022, 43(7): 965-972.
［1］Kouretas M, Tsatsakis A, Koureas M,et al. Systematic review of biomonitoring studies to determine the assocication between exposure to organophosphorus and prethroid insecticidies and human health outcomes ［J］. Toxicology Letters, 2011, 210 (2): 155-168.
［2］Mostafalou S, Abdollahi M. Pesticides: An update of human exposure and toxicity ［J］. Arch Toxicol, 2017, 91 (2): 549-599.
［3］翟洪稳, 范素芳, 王娟, 等. 测量不确定度在食品检验中的应用及进展 ［J］. 食品科学, 2021,42(5):314-320.
Zhai H W, Fan S F, Wang J, et al. Application and progress of measurement uncertainty in food inspection and detection ［J］. Food Science,2021,42(5):314-320.
［4］王海滨, 陈雪宁, 于海滨. 食品检验在保障食品安全中的重要性及其局限性 ［J］. 现代食品, 2019(11): 112-113+116.
Wang H B, Chen X N, Yu H B. Importance and Limitation of Food Inspection in Safeguarding Food Safety ［J］. Modern Food, 2019(11): 112-113+116.
［5］李培武, 张奇, 丁小霞, 等. 食用植物性农产品质量安全研究进展 ［J］. 中国农业科学, 2014, 47 (18): 3618-3632.
Li P W, Zhang Q, Ding X X, et al. A Review of Studies on Quality and Safety of Edible Vegetable Agro-Products ［J］. Scientia Agricultura Sinica, 2014, 47(18): 3618-3632.
［6］CAC/GL 59-2006 Guidelines on estimation of uncertainty of results［S］.
［7］王宏涛, 王汉斌, 陈晓怀, 等. 测量不确定度引起的批量产品检验误判风险评估 ［J］. 计量学报, 2017, 38 (5): 559 -562.
Wang H T, Wang H B, Chen X H, et al. Evaluation of misjudgment risks caused by measurement uncertainty for batch product inspection ［J］. Acta Metrologica Sinica, 2017, 38 (5): 559-562.
［8］李德恒,陆晶芳,曾金林, 等.液相色谱串联质谱法测定鸡蛋中利巴韦林及其代谢物总残留的不确定度评定 ［J］. 计量学报, 2021, 42(9): 1250-1256.
Li D H, Lu J F, Zeng J L,et al.Evaluation of Uncertainty in Determination of Total Residues of Ribavirin and its Metabolites in Eggs by LC-MS/MS［J］. Acta Metrologica Sinica, 2021, 42(9): 1250-1256.
［9］殷朝珍, 翟付凤, 董卫峰. 气相色谱法测定蔬菜中有机磷农药残留量不确定度评定研究 ［J］. 现代农业科技, 2014 (17): 153-155.
Yin C Z, Zhai F F, Dong W F. Uncertainty Evaluation of Organic Phosphorus Pesticide Residues in Vegetables Determined by GC ［J］. Modern Agricultural Science and Technology, 2014 (17): 153-155.
［10］洪泽淳, 熊含鸿, 刘莹莹, 等. 气相色谱法测定蔬菜中16种有机磷农药残留量不确定评定 ［J］. 食品工业科技, 2020(3): 239-245.
Hong Z C, Xiong H H, Liu Y Y, et al. Evaluation of Measurement Uncertainty in the Determination of 16 Organophosphorus Pesticide Residues in Vegetables by Gas Chromatography ［J］. Science and Technology of Food Industry, 2020(3): 239-245.
［11］王璐, 贺泽英, 罗铭, 等. 蔬菜中农药残留测定的测量不确定度评定 ［J］. 安徽农业科学, 2015, 43 (3): 113-115+119.
Wang L, He Z Y, Luo M, et al. Measurement Uncertainty Evaluation of Determination Pesticide Residues in Vegetables ［J］. Journal of Anhui Agricultural Sciences, 2015, 43 (3): 113-115+119.
［12］柴宗龙, 袁彩霞, 周鑫魁, 等. 气相色谱法测定黄瓜中丙溴磷农药残留量的测定不确定度评定 ［J］. 食品工业科技,2020,41(12):238-244.
Chai Z L, Yuan C X, Zhou X K, et al. Measurement Uncertainty was Evaluated in Determination of Profenofos (PFF) Residues in Cucumber by Gas Chromatography (GC) ［J］. Science and Technology of Food Industry, 2020,41(12):238-244.
［13］贺玲, 段书源, 戴崔云, 等. 气相色谱法测定普通白菜中毒死蜱含量的不确定度 ［J］. 食品安全质量检测学报, 2019, 10 (10): 3085-3090.
He L, Duan S Y, Dai C Y, et al. Uncertainty evalua-tion of determination of chlorpyrifos pesticide residues in common Chinese cabbage-pak-choi by Gas Chromatography ［J］. Journal of Food Safety and Quality, 2019, 10 (10): 3085-3090.
［14］罗彦平, 单江华, 高海文, 等. 番茄中联苯菊酯残留量的测定不确定评价 ［J］. 中国计量大学学报, 2017, 28 (4): 424-429.
Luo Y P, Shan J H, Gao H W, et al. Evaluation of measurement uncertainty of bifenthrin residues in tomato fruits ［J］. Journal of China University of Metrology, 2017, 28 (4): 424-429.
［15］CNAS-GL006: 2018 化学分析中不确定度的评估指南化学分析中不确定度的评估指南［S］.
［16］JJF 1059. 1—2012 测量不确定度评定与表示［S］.
［17］陈凌峰. 标准不确定度 A 类评定中极差法的深入讨论 ［J］. 计量学报, 2019, 40 (2): 347-352.
Chen L F. The Further Discussion of the Range Method in the Type A Evaluation of Sstandard Uncertainty ［J］. Acta Metrologica Sinica, 2019, 40 (2): 347-352.
［18］陈凌峰. 抽样引起的测量不确定度评定 ［J］. 计量学报, 2020, 41(7): 891-896.
Chen L F.Evaluating the Sampling Contribution to the Measurement Uncertainty［J］. Acta Metrologica Sinica, 2020, 41(7): 891-896.
［19］JJG 196—2006 常用玻璃量器检定规程［S］. 2006.
［20］JJG 1036—2008 电子天平检定规程［S］. 2006.
［21］黄荣浪, 章虎, 王祥云, 等. 气相色谱法测定蔬菜中有机磷农药残留的测量不确定度 ［J］. 安徽农业科学, 2010, 38 (13): 7124-7127.
Huang R L, Zhang H, Wang X Y, et al. Measure Uncertainty of measuring organic phosphorous pesticide residue in vegetables with GC［J］. Journal of Anhui Agricultural Sciences, 2010, 38 (13): 7124-7127.
［22］汪志威, 周思齐, 李非里, 等. 实验室农药残留检测的测量不确定度评定—以 GB 23200.8—2016 测定草莓中 4种农药残留为例［J］. 农药学学报, 2020, 22(1): 105-114.
Wang Z W, Zhous Q, Li F L, et al. Evaluating the uncertainty of measurement of pesticide residue detection:a case study of four pesticide residues in strawberry by GB 23200.8—2016［J］. Chinese Journal of Pesticide Science, 2020, 22(1): 105-114.
［23］方学智, 费学谦, 丁明, 等. 玉米中氯氰菊酯、溴氰菊酯 SPE 净化及不确定度分析 ［J］. 农药, 2009, 48 (2): 127-129.
Fang X Z, Fei X Q, Ding M, et al. Purification of Permethrin and Deltamethrin in Maize by SPE and Evaluation of Uncertainty ［J］. Agrochemicals, 2009, 48 (2): 127-129.
［24］王高俊, 吴昊, 章明洪.自适应蒙特卡洛法评定肥料中苯并［a］芘含量的测量不确定度［J］. 计量学报, 2022, 43(1): 127-132.
Wang G J, Wu H, Zhang M H. Evaluation of Measurement Uncertainty in the Determination of Benzo［a］pyrene in Fertilizer by Adaptive Monte Carlo Method［J］. Acta Metrologica Sinica, 2022, 43(1): 127-132.
2022, Vol. 43 
