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Analysis of pesticide residues in melon using QuEChERS extraction and liquid chromatography triple quadrupole mass spectrometry

机译:QuEChERS萃取和液相色谱三重四极杆质谱法分析瓜中的农药残留

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摘要

A rapid, precise and efficient method for the determination of seven insecticides (chlorpyrifos, dimethoate, deltamethrin, thiamethoxam, thiacloprid, pirimicarb and indoxacarb) and three fungicides (azoxystrobin, fluopicolide and propamocarb hydrochloride) in melon by employing quick, easy, cheap, effective, rugged and safe extraction method coupled with liquid chromatography triple quadrupole mass spectrometry was developed and validated by evaluating the accuracy, precision, linearity, limit of detection (LOD) and limit of quantification (LOQ). The average recoveries of the selected pesticides ranged from 82% to 106% with RSDr 6% in four fortification levels of 0.01, 0.05, 0.1 and 0.2mg/kg. The correlation coefficient (R-2) was 0.997 for all the selected pesticides when matrix-matched calibration standards were used. The LOD values ranged from 0.001 to 0.003mg/kg, and the LOQ was determined at 0.01mg/kg for all the analytes. Matrix effect was evaluated, and it was found considerable for thiamethoxam and deltamethrin (-53% and +135%, respectively). Finally, this method was applied for the residue analysis of 122 fresh melon samples collected from different market places in Thessaloniki, Greece. Among the 122 analysed samples, 32 (26% of the total no. of samples) were found to have pesticide residues. None of the samples contained residues above the European Union-Maximum Residue Levels. The most frequently detected pesticides were fluopicolide and thiamethoxam.
机译:一种快速,准确,高效的方法,可快速,简便,廉价,有效地测定瓜中的七种杀虫剂(毒死rif,乐果,溴氰菊酯,噻虫嗪,噻虫啉,吡虫威和吡虫威)和三种杀真菌剂(氮氧嘧菌酯,氟吡草胺和盐酸丙氨威)。通过评估准确度,精密度,线性,检测限(LOD)和定量限(LOQ),开发并验证了耐用安全的萃取方法与液相色谱三重四极杆质谱联用。所选农药的四种强化水平分别为0.01、0.05、0.1和0.2mg / kg,平均回收率在82%至106%之间,RSDr为6%。当使用基质匹配的校准标样时,所有选定农药的相关系数(R-2)为0.997。 LOD值在0.001至0.003mg / kg的范围内,所有分析物的LOQ被确定为0.01mg / kg。对基质效应进行了评估,发现噻虫嗪和溴氰菊酯具有显着效果(分别为-53%和+ 135%)。最后,该方法用于从希腊萨洛尼卡不同市场收集的122个新鲜瓜样品的残留分析。在122个被分析的样品中,有32个(占样品总数的26%)被发现具有农药残留。样品中均未包含高于欧盟最大残留限量的残留。检出率最高的农药是氟吡考特和噻虫嗪。

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