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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。
In order to meet the needs of agricultural products and food safety testing, this paper verifies the suitability of GB / T 20769-2008 for the determination of flurbaronitrile residues in cantaloupe and eggplant samples and simplifies the pretreatment steps. Samples of fruits and vegetables were extracted with acetonitrile and extracted by solid-liquid extraction using acetonitrile as extractant. The mixture was purified by salting-out and column chromatography using methanol-dichloromethane (5:95, v : V) Elution of nitrofluorfenonitrile in methanol, water (1: 1, v: v), over 0.2 μm filter; analysis in UPLC-MS / MS anion scan multiple reaction monitoring mode . The linear correlation coefficients (r = 0.9998 and 0.9992) of flurbarum nitrile between the two substrates of cantaloupe and eggplant were 0.9998 and 0.9992, respectively. The recoveries of the two methods were 81.00% ~ 107.76% at RSD of 2.56% ~ 3.82% at three levels of 500, 200 and 50 μg / L. The detection limit of detection (LOD) was 0.72 μg / kg and 0.62 μg / kg. The accuracy and precision of the method are in line with the requirements of residue analysis. The method is efficient, rapid, simple, sensitive, confirmatory and practical. It is applicable to the conventional method for the detection of residual residues of flurbaron in cantaloupe and eggplant.