气相色谱-质谱联用检测烟草中拟除虫菊酯类农药残留量的不确定度评定  

Uncertainty Evaluation for Determination of Pyrethroid Pesticide Residues in Tobacco by Gas Chromatograph-Mass Spectrometry

作　　者：袁芳 刘小艳 姚明月 肖新生 李佳颖 陈馨 YUAN Fang;LIU Xiaoyan;YAO Mingyue;XIAO Xinsheng;LI Jiaying;CHEN Xin(Yongzhou Tobacco Company of Hu’nan Province,Yongzhou,Hu’nan 425100,China;China College of Chemistry and Bioengineering,Hu’nan University of Science and Engineering,Yongzhou,Hu’nan 425199,China;Daoxian Branch of Yongzhou Tobacco Company of Hu’nan Province,Yongzhou,Hu’nan 425300,China)

机构地区：[1]湖南省烟草公司永州市公司,湖南永州425100 [2]湖南科技学院化学与生物工程学院,湖南永州425199 [3]湖南省烟草公司永州市公司道县分公司,湖南永州425300

出　　处：《热带农业科学》2024年第4期73-83,共11页Chinese Journal of Tropical Agriculture

基　　金：湖南省烟草公司永州市公司2022年度烟叶科研项目计划(永烟技[2022]17号)。

摘　　要：依据行业标准YC/T 405.3—2011,采用气相色谱-质谱联用对烟草中拟除虫菊酯类农药的残留量进行了不确定度评定,通过建立测量模型,识别和量化实验过程中的不确定度来源,接着对各不确定度分量进行合成和扩展,最终得出6种农药的实际检测结果。结果表明,影响不确定度的主要因素为标准溶液配制、标准曲线拟合,其次为测量重复性和样品制备,回收率对不确定度的影响相对较小;在95.45%置信区间时,取包含因子k=2,烟草中氟氯氰菊酯、氯菊酯、高效氯氟氰菊酯、氯氰菊酯、氰戊菊酯、溴氰菊酯的检测结果及扩展不确定度分别为(0.4810±0.0402)、(0.4660±0.0397)、(1.0359±0.1024)、(1.0147±0.1012)、(0.9400±0.0759)、(0.9490±0.0770)mg/kg;标准溶液配制对6种农药引入的不确定度分量贡献率为40%~60%,而样品制备和回收率对6种农药引入的不确定度分量贡献率普遍较低,为2%~9%。为了减小不确定度应该配制合适浓度的标准溶液,优化样品制备过程中的前处理步骤,提高人员的实验操作能力,定期对仪器及量具进行维护。According to the industry standard YC/T 405.3-2011,the uncertainty of pyrethroid pesticide residues in tobacco was evaluated by using gas chromatography-mass spectrometry.By establishing the measurement model,identifying and quantifying the sources of uncertainty during the experiment,and then synthesizing and expanding the components of uncertainty,the actual test results of six pesticides were finally obtained.The results showed that the main factors affecting the uncertainty were standard solution preparation and standard curve fitting,followed by measurement repeatability and sample preparation,and the recovery rate had relatively little effect on the uncertainty.With a confidence of 95%and a coverage factor of k=2,the measurement results and expanded uncertainty of cypermethrin,permethrin,beta-cyhalothrin,cypermethrin,valerthrin,and deltamethrin in tobacco were(0.4810±0.0402),(0.4660±0.0397),(1.0359±0.1024),(1.0147±0.1012),(0.9400±0.0759),(0.9490±0.0770)mg·kg–1,respectively.The contribution rate of standard solution preparation to the uncertainty component of the six pesticides ranged from 40%to 60%.However,the contribution rate of sample preparation and recovery to the uncertainty component of the six pesticides was generally low,ranging from 2%to 9%.It is necessary to prepare the standard solution at an appropriate concentration,optimize the pre-treatment steps in the sample preparation process,improve the experimental operation ability of personnel,and maintain the instrument and measuring tool regularly to reduce uncertainty.

关 键 词：烟草 不确定度 气相色谱-质谱联用 拟除虫菊酯类农药 

分 类 号：S572[农业科学—烟草工业]