Determination of sulfoxaflor residues in melon and eggplant by ultra-high performance liquid chromatography-tandem mass spectrometry
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摘要: 为满足农产品与食品安全检测的需求,本文验证GB/T 20769-2008对哈密瓜和茄子样品中氟啶虫胺腈残留量测定的适用性并简化前处理步骤。果蔬样品用乙腈为提取剂,采用组织捣碎、固液提取法提取果蔬中的氟啶虫胺腈,通过盐析离心,氨基柱固相萃取净化,甲醇∶二氯甲烷（5∶95,v∶v）洗脱样品中的氟啶虫胺腈,甲醇∶水（1∶1,v∶v）定容,过0.2μm滤膜;在UPLC-MS/MS负离子扫描多反应监测模式下进行分析。氟啶虫胺腈在哈密瓜与茄子两种基质中的线性相关系数r分别为0.9998和0.9992。在500、200、50μg/L三个添加水平下的回收率为81.00%107.76%,RSD在2.56%3.82%范围内,方法检出限（LOD）在哈密瓜与茄子中分别为0.72μg/kg与0.62μg/kg。该方法的准确度和精密度均符合残留分析的要求,而且高效、快速、简单、灵敏度高、确认性和实用性强,适用于氟啶虫胺腈在哈密瓜、茄子残留检测的常规方法。
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关键词:
- 氟啶虫胺腈 /
- 超高效液相色谱-串联质谱法 /
- 茄子 /
- 哈密瓜 /
- 残留量
Abstract: It is verified that GB/T 20769-2008 is also suitable for the determination of the residue of sulfoxaflor in the samples of cantaloupe and eggplant and simplied the pretreatment steps. Samples of melon and eggplant were initially extracted with acetonitrile, salting out by Na Cl, cleaned up by aminopropyl ( NH2) cartridge, eluted by methanol and dichloromethane ( 5∶ 95, v∶ v) , metered by methanol and water ( 1 ∶ 1, v ∶ v) . After filtered with a 0.2 μm membrane, the resulting samples determined by UPLC-MS/MS performing on negative electrospray ionization and the multiple reactions monitoring mode ( MRM) .The matrix-matched external standard calibration curves were used for quantitative analysis.The linearly dependent coefficient r of sulfoxaflor for cantaloupe and eggplant were 0.9998 and 0.9992, respectively.The added recoveries were between81.00% 107.76% in the concentration range of 50 ~ 500 μg/L. The lowest limit of detection ( LOD) was 0.72 μg/kg and0.62 μg/kg, and the relative standard deviations ( RSD, n = 6) were in the range of 2.56% ~ 3.82%. The method can meet the requirements for determination of sulfoxaflor residue in cantaloupe and eggplant, and it is a quick, easy, effective, sensitive and accurate method. -
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