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采用 GC-ECD 对果蔬中有机氯和拟除虫菊酯类农药残留的 QuEChERS 分析技术进行验证。

Validation of QuEChERS analytical technique for organochlorines and synthetic pyrethroids in fruits and vegetables using GC-ECD.

机构信息

Department of Entomology, Dr. Y.S. Parmar University of Horticulture and Forestry, Nauni, Solan, HP, 173230, India.

College of Horticulture and Forestry, Neri, PO Khaggal, District Hamirpur HP, 177001, India.

出版信息

Environ Monit Assess. 2018 Mar 19;190(4):231. doi: 10.1007/s10661-018-6584-8.

Abstract

In the present day scenario of increasing awareness and concern about the pesticides, it is very important to ensure the quality of data being generated in pesticide residue analysis. To impart confidence in the products, terms like quality assurance and quality control are used as an integral part of quality management. In order to ensure better quality of results in pesticide residue analysis, validation of analytical methods to be used is extremely important. Keeping in view the importance of validation of method, the validation of QuEChERS (quick, easy, cheap, effective, rugged, and safe) a multiresidue method for extraction of 13 organochlorines and seven synthetic pyrethroids in fruits and vegetables followed by GC ECD for quantification was done so as to use this method for analysis of samples received in the laboratory. The method has been validated as per the Guidelines issued by SANCO (French words Sante for Health and Consommateurs for Consumers) in accordance with their document SANCO/XXXX/2013. Various parameters analyzed, viz., linearity, specificity, repeatability, reproducibility, and ruggedness were found to have acceptable values with a per cent RSD of less than 10%. Limit of quantification (LOQ) for the organochlorines was established to be 0.01 and 0.05 mg kg for the synthetic pyrethroids. The uncertainty of the measurement (MU) for all these compounds ranged between 1 and 10%. The matrix-match calibration was used to compensate the matrix effect on the quantification of the compounds. The overall recovery of the method ranged between 80 and 120%. These results demonstrate the applicability and acceptability of this method in routine estimation of pesticide residues of these 20 pesticides in the fruits and vegetables by the laboratory.

摘要

在当今人们对农药的认识和关注日益提高的情况下,确保农药残留分析中生成的数据质量非常重要。为了使产品更具信心,人们将质量保证和质量控制等术语用作质量管理的一个组成部分。为了确保在农药残留分析中获得更好的结果质量,对拟使用的分析方法进行验证非常重要。鉴于方法验证的重要性,对 QuEChERS(快速、简单、廉价、有效、耐用和安全)多残留方法进行了验证,该方法用于提取水果和蔬菜中的 13 种有机氯农药和 7 种合成拟除虫菊酯,然后用 GC ECD 进行定量分析,以便在实验室中使用该方法分析收到的样品。该方法已按照 SANCO(法语单词 Sante 表示健康,Consommateurs 表示消费者)发布的指南进行验证,符合其文件 SANCO/XXXX/2013。分析了各种参数,即线性、特异性、重复性、重现性和稳健性,发现其值均在可接受范围内,相对标准偏差(RSD)小于 10%。有机氯农药的定量下限(LOQ)设定为 0.01 和 0.05mg/kg,合成拟除虫菊酯的定量下限(LOQ)设定为 0.01 和 0.05mg/kg。所有这些化合物的测量不确定度(MU)在 1%至 10%之间。使用基质匹配校准来补偿化合物定量时的基质效应。该方法的总体回收率在 80%至 120%之间。这些结果表明,该方法可用于实验室常规估计这些 20 种农药在水果和蔬菜中的残留量,适用性和可接受性良好。

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