超高效液相色谱-串联质谱法同时测定水产品中6种丁香酚类物质的残留量

Determination of 6 Eugenol Residues in Aquatic Products by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

建立同时测定水产品中丁香酚、异丁香酚、甲基丁香酚、甲基异丁香酚、乙酸丁香酚酯、乙酰基异丁香酚的超高效液相色谱-串联质谱(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)方法,并应用于实际样品的测定。样品加入无水硫酸钠进行基质分散后以乙腈振荡提取,提取液经HLB固相萃取柱净化,浓缩后,以Shim-pack GIST(2.1 mm×50 mm,2μm)为色谱柱,甲醇-水作为流动相进行梯度洗脱分离,UPLC-MS/MS进行分析。方法学验证表明,在1.00~500 ng/mL范围内,6种丁香酚类物质线性关系较好(R>0.999);检出限在0.1~0.3μg/kg之间;定量限在0.3~1.0μg/kg之间;以3种不同基质进行2.00、5.00、10.0μg/kg的加标回收实验,每种加标水平平行实验6次。结果显示6种丁香酚类物质平均回收率在83.9%~105.4%之间,相对标准偏差在1.8%~6.9%之间,符合痕量分析的要求。该法简便、结果准确可靠、灵敏度高、检出限低,适用于水产品中6种丁香酚类物质的测定。

A new method for simultaneous determination of eugenol,isoeugenol,methyl eugenol,methyl isoeugenol,aceteugenol and lsoeugenyl acetate residues in aquatic products by ultra-high performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS)was developed.The samples were extracted with acetonitrile and purified on an HLB solid phase extraction(SPE)column.Chromatographic separation was achieved on a Shim-pack GIST column(2.1 mm×50 mm,2μm)by linear gradient elution using methanol/water as the mobile phase before analysis by UPLCMS/MS.The method validation showed that good linearity(R>0.999)was observed in the range of 1.00–500 ng/mL for the 6 eugenols.The limits of detection(LODs)were between 0.1 and 0.3μg/kg,and the limits of quantification(LOQs)were between 0.3 and 1.0μg/kg.The recoveries ranged between 83.9%and 105.4%at three spiked levels(2.00,5.00,and 10.0μg/kg)with relative standard deviations(n=6)between 1.8%and 6.9%.This method proved to be simple,accurate,sensitive,and suitable for the quantitative determination of six eugenol residues in aquatic products.