高效液相色谱法测定苹果中多菌灵残留量的测量不确定度分析
投稿时间:2009-12-21   修订日期:2010-03-25   点此下载全文 HTML
引用本文:杨媛,石磊,李文生,等.高效液相色谱法测定苹果中多菌灵残留量的测量不确定度分析[J].农药学学报,2010,12(3):349-354.
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作者单位E-mail
杨媛 北京市农林科学院 林业果树研究所北京 100093  
石磊 北京市农林科学院 林业果树研究所北京 100093  
李文生 北京市农林科学院 林业果树研究所北京 100093  
王宝刚 北京市农林科学院 林业果树研究所北京 100093  
冯晓元 北京市农林科学院 林业果树研究所北京 100093 xyfeng@yahoo.cn 
张开春 北京市农林科学院 林业果树研究所北京 100093  
王纪华 北京农产品质量检测与农田环境监测技术研究中心北京 100097  
基金项目:北京市科委科技计划 (Z09090501040901)
中文摘要:建立了评定NY/T 1680-2009“蔬菜水果中多菌灵等4种苯并咪唑类农药残留量的测定——高效液相色谱法”中影响测量不确定度的各因素的数学模型,考察了样品前处理和液相色谱测定的各个环节,并根据所建立的数学模型计算了评定测量不确定度的各分量。采用该方法测得市售苹果中多菌灵的残留量为0.23 mg/kg。分析表明:多菌灵残留量测定的不确定度主要来源于样品溶液的平行测定、样品稀释以及萃取、净化等处理过程产生的回收率差异;此外,标准溶液的配制和检测过程以及提取处理等其他环节对其也有一定影响。经计算,在置信概率P=95%时,采用该方法测定试样中多菌灵残留的扩展不确定度为0.02 mg/kg,若不考虑多菌灵残留在样品中分布的均匀性,则苹果试样中多菌灵残留的检测结果可表示为(0.23±0.02) mg/kg(包含因子k=2)。
中文关键词:高效液相色谱  苹果  多菌灵  残留  测量不确定度
 
Evaluation of uncertainty in measurement of carbendazim residue in apple determined by high performance
Abstract:According to the method of NY/T 1680-2009 “Determination of carbendazim and other 3 benzimidazoles in vegetable and fruit by HPLC”,the mathematical model was established and used to evaluate the uncertainty in the measurement of carbendazim residue in apple.Every link of sample pretreatment and HPLC determination was analyzed,and then the uncertainty components were calculated on the basis of mathematical model.The determination result showed that concentration of carbendazim residue in sample was 0.23 mg/kg.The uncertainty in measurement of carbendazim residue mainly originated from recovery rate in parallel determination of sample solution by HPLC,dilution process of sample solution,extraction and purification of sample.Moreover,other processes,such as preparation,detection and extraction of standard solution by HPLC,had some influence on the uncertainty.When the confidence probability was 95%,the extended uncertainty in measurement of carbendazim residue in apple by HPLC was 0.02 mg/kg.So the carbendazim residue in test sample can be expressed as (0.23±0.02) mg/kg (k=2) in case that the distribution of residue in apple be not considered at this circumstance.
Key words:HPLC  vegetable  apple  residue  uncertainly of measurement
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