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作 者:胡西洲[1] 彭西甜[1] 张仙[1] 夏虹[1] 周有祥[1] 彭立军[1] 孙丹陵 HU Xizhou;PENG Xitian;ZHANG Xian;XIA Hong;ZHOU Youxiang;PENG Lijun;SUN Danling(Institute of Quality Standards and Testing Technology for Agro-Products,Hubei Academy of Agricultural Sciences,Hubei Key Laboratory of Nutritional Quality and Safety of Agro-Products,Wuhan 430064,China;College of Laboratory Medicine,Hubei University of Chinese Medicine,Wuhan 430065,China)
机构地区:[1]湖北省农业科学院农业质量标准与检测技术研究所,湖北省营养品质与农产品安全重点实验室,武汉430064 [2]湖北中医药大学检验学院,武汉430065
出 处:《分析试验室》2022年第10期1174-1179,共6页Chinese Journal of Analysis Laboratory
基 金:湖北省重点研发计划(2020BBB078)项目资助。
摘 要:在复杂基质的农药多残留分析中,常采用标准曲线进行外部校准。溶剂校准法仅适用于基质效应较小的样品溶液的校正;尽管基质匹配校准法可以补偿基质效应,但不能补偿过程损失。标准添加法和程序标准校准法可以补偿过程损失,然而需要更多的样品和/或基质空白、更多的样品制备时间和成本。因此,建立了一种稀释标准添加校准法,结合QuEChERS法和气相色谱串联质谱用于黄瓜中19种常见农药残留量的快速测定。结果表明,该方法回收率为85.7%~105.9%,相对标准偏差(RSD)为0.8%~8.5%,测定不确定度平均值为13.6%。对基质效应、准确度、精密度、不确定度和适用性等进行了考察,为农药多残留快速准确分析提供支撑。External calibration based on the standard curve was usually adopted in pesticides multi-residues analysis in complex sample matrices. Solvent calibration was merely suitable for the calibration of sample solutions with small matrix effects. Although matrix matched calibration could compensate for matrix effects,while it could not compensate for process losses. Meanwhile, although standard addition methods and procedural standard calibration methods can compensate for process losses, more samples and/or matrix blanks, more sample preparation time and cost are required. To solve this problem, a dilution standard addition calibration method was established with QuEChERS method and gas chromatography tandem mass spectrometry for the determination of 19 common pesticide residues in cucumber. The results showed that the recovery rates were 85.7%-105.9% with the relative standard deviations(RSDs)of 0.8%-8.5%,and the average measurement uncertainty of 13.6%.Several related parameters such as matrix effect,accuracy,precision,uncertainty and applicability were investigated to provide support basis for the rapid and accurate analysis of the pesticide multi-residue analysis.
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