摘要
为建立芹菜根、茎、叶中吡虫啉、唑螨酯残留的Qu ECh ERS-LC-MS/MS分析方法,采用Qu ECh ERS方法对样品进行提取和净化,通过液相色谱-串联三重四极杆质谱联用仪(LC-MS/MS)测定样品中吡虫啉、唑螨酯残留。结果表明:添加质量分数为0.05~1.00 mg·kg^(-1)时,吡虫啉在芹菜根、茎、叶中的平均添加回收率为77.15%~103.48%,RSDs为1.40%~9.97%;唑螨酯在芹菜根、茎、叶中的平均添加回收率为77.35%~100.42%,RSDs为2.01%~6.95%。吡虫啉、唑螨酯的检出限(LODs)分别是0.120、0.015μg·kg^(-1);吡虫啉在芹菜根、茎、叶的定量限(LOQs)分别为1.65、0.87、1.08μg·kg^(-1);唑螨酯在芹菜根、茎、叶的LOQs分别是1.24、0.75、0.78μg·kg^(-1)。该方法操作简单,回收率、精密度均符合农药残留分析的要求,适合实验室大量样品的检测。
In this study,a simple and practical Qu ECh ERS-liquid chromatography-tandem mass spectrometry( LCMS/MS) method was established to detect the residues of imidacloprid and fenpyroximate in the roots,stems,leaves of celery. The samples were extracted and purified by Qu ECh ERS method,and analyzed by LC-MS/MS. Results showed that the average recoveries of imidacloprid in roots,stems,leaves of celery were 77. 15%-103. 48% at three spiking levels from 0. 05 mg·kg^(-1) to 1. 00 mg·kg^(-1) with relative standard deviations( RSDs) of 1. 40%-9. 97%. The average recoveries of fenpyroximate in roots,stems,leaves of celery were 77. 35%-100. 42% at three spiking levels from 0. 05 mg·kg^(-1) to 1. 00 mg·kg^(-1) with relative standard deviations( RSDs) of 2. 01%-6. 95%.Limit of detections( LODs) were estimated to be 0. 120 μg·kg^(-1) for imidacloprid,and 0. 015 μg·kg^(-1) for fenpyroxi-mate,respectively. Limit of quantitations( LOQs) for imidacloprid in the roots,stems,leaves of celery were 1. 65,0. 87 and 1. 08 μg·kg^(-1),respectively. LOQs for fenpyroximate were 1. 24 μg·kg^(-1)( roots),0. 75 μg·kg^(-1)( stems)and 0. 78 μg·kg^(-1)( leaves). The celery samples were detected using this established method,the recovery and the precision were in accordance with the requirements of pesticide residue analysis. The method was suitable for the detection of a large number of samples in the laboratory.
出处
《浙江农业学报》
CSCD
北大核心
2018年第2期261-267,共7页
Acta Agriculturae Zhejiangensis
基金
国家重点研发项目子课题(2016YFD0200204-)
公益性行业(农业)科研专项经费项目(201503107-12)