固相萃取-高效液相色谱-串联质谱法测定蜂蜜中残留的酞丁安

Determination of Ftibamzone in Honey by Solid Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry

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,2.7μm)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5μg/L~1 000μg/L范围内线性关系良好(R^(2)> 0.99),酞丁安的检出限和定量限分别为2、5μg/kg。酞丁安在蜂蜜样品中添加水平为5、50、200μg/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。

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,2.7 μm)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(R^(2)> 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.