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投稿时间:2020-08-12
投稿时间:2020-08-12
中文摘要: 该研究采用固相萃取-高效液相色谱-质谱联用技术(high performance liquid chromatography-mass spectrometry coupled with solid phase extraction,SPE-LC-MS/MS)结合固相萃取净化法,建立蜂蜜中残留酞丁安的定量分析方法。蜂蜜样品经水溶解并振荡提取,离心除去杂质后,由PH苯基固相萃取小柱富集净化,以0.1%甲酸-水溶液和乙腈为流动相,采用C18色谱柱(3.0 mm×100 mm,2.7 μm)进行梯度洗脱分离,在正离子模式下,采用多反应监测模式检测。结果表明,酞丁安在5 μg/L~1 000 μg/L范围内线性关系良好(R2>0.99),酞丁安的检出限和定量限分别为2、5 μg/kg。酞丁安在蜂蜜样品中添加水平为5、50、200 μg/kg时,添加回收率为93.67%~99.61%,日内和日间相对标准偏差(relative standard deviation,RSD)分别为2.74%~4.73%和2.3%~3.87%(n=6)。该方法适用于蜂蜜中酞丁安残留筛查检测及定量分析,可为其他食品中酞丁安残留测定分析提供方法指导。
中文关键词: 蜂蜜 酞丁安 高效液相色谱-三重四极杆串联质谱 固相萃取 提取剂
Abstract:A method combining liquid chromatography-mass spectrometry with solid phase extraction was established for the determination of ftibamzone resdue in honey.The honey samples were dissolved in distilled water and purified using solid phase extraction with a phenyl column.The target compound was separated using a gradient elution process with a C18 column(3.0 mm× 100 mm,2.7μm)with two mobile phases consisting of 0.1% formic acid aqueous solution and acetonitrile.The quantitative detection was performed using an electrospray ionization source in positive ionization mode under multiple reaction monitoring mode.The standard curve was constructed and exhibited a strong linear response (R2>0.99)in the range of 5 μg/L-1 000 μg/L.The limit of detection for ftibamzone in honey was 2 μg/kg,and the limit of quantification was 5 μg/kg.The recoveries ranged from 93.67% to 99.61%,with intraday relative standard deviation of 2.74%-4.73% and inter-day relative standard deviation of 2.3%-3.87% at three spiked levels(5,50,200 μg/kg)in blank honey samples(n=6).The method developed in this study was suitable for the rapid detection of ftibamzone residue in honey and could provide a reference for ftibamzone analysis in other foods.
keywords: honey ftibamzone high performance liquid chromatography-tandem mass spectrometry (HPLCMS/MS) solid phase extraction(SPE) extracting agent
文章编号:202114023 中图分类号: 文献标志码:
基金项目:国家蜂产业技术体系(CARS-44-KXJ8);国家特色农产品风险评估专项(GJFP2020010);中国农业科学院创新工程项目(CAASASTIP-2020-IAR)
作者 | 单位 |
王玉涵,王欣然,李熠,周金慧 | 中国农业科学院蜜蜂研究所,北京 100093;农业农村部蜂产品质量安全控制重点实验室,北京 100093;农业农村部蜂产品质量安全风险评估实验室(北京),北京 100093;农业农村部蜂产品质量监督检验测试中心(北京),北京 100093 |
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