摘要
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.
作者
吴少明
蔡小明
周鹏
蔡慧钦
梁敏
陈言凯
李燕平
冯丽凤
林浩学
黄媛
WU Shaoming;CAI Xiaoming;ZHOU Peng;CAI Huiqin;LIANG Min;CHEN Yankai;LI Yanping;FENG Lifeng;LIN Haoxue;HUANG Yuan(Fujian Inspection and Research Institute for Product Quality,China National Quality Supervision and Testing Center for Processed Food,Fuzhou 350002,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2020年第16期320-326,共7页
Food Science
基金
福建省产品质量检验研究院科技项目(KY201813A)。
关键词
超高效液相色谱-串联质谱
丁香酚
固相萃取
水产品
ultra-high performance liquid chromatography-tandem mass spectrometry
eugenol
solid-phase extraction
aquatic products