食品工业科技2024，Vol.45Issue(1)：284-294,11.DOI:10.13386/j.issn1002-0306.2023030164
SPE-UPLC-MS/MS同时测定食品中24种酸性工业染料
Simultaneous Determination of 24 Acid Industrial Dyes in Food by Solid Phase Extraction-Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A method based on solid phase extraction(SPE)combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established for the determination of 24 acid industrial dyes in food.The sample was extracted with ammonia-ethanol solution(ammonia:absolute ethyl alcohol:water=2:7:1,v/v),the extracting solution was condensed to 1 mL under a stream of nitrogen,then dissolved by 10 mL 5%methanol-water solution.The solution was purified by Agela Cleanert PWAX SPE column.The eluant was dried with nitrogen and dissolved by ammonium acetate acetonitrile solution(10 mmol/L ammonium acetate water:acetonitrile =1:1,v/v),the analytes were separated by the Agilent ZORBAX Eclipse RRHD C18(3.0 mm×150 mm,1.8 μm)column using mobile phase gradient with acetonitrile and 10 mmol/L ammonium acetate.The analytes were ionized with negative electrospray ionization(ESI-)and analyzed by multiple reaction monitoring(MRM)mode,then quantified by external standard method.The linearity of 24 acid industrial dyes displayed good linearities in the range from 20～300 ng/mL,the correlation coefficients higher than 0.999.The limits of detection(LOD)and quantification(LOQ)were 10 μg/kg and 25 μg/kg.The recoveries at three level spiked levels(25、100、250 μg/kg)were 91.0%～112.7%with the relative standard deviations(n=6)between 0.42%and 4.39%.The method was applied to determine 40 batches of bean products,condiments,aquatic products and meat products each,the acid orange Ⅱwas detected in 2 batches of braised meat samples,the content was 138±2.8 μg/kg and 179±3.7 μg/kg,the red 2G was detected in 2 batches of sausage samples,the content was 320±8.6 μg/kg and 230±6.2 μg/kg.The method is rapid,sensitive and reliable,it can be applied to determine 24 acid industrial dyes in food.关键词
酸性工业染料/固相萃取(SPE)/超高效液相色谱-串联质谱(UPLC-MS/MS)/豆制品/调味品/水产品/肉制品Key words
acid industrial dyes/solid phase extraction(SPE)/ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)/bean products/condiments/aquatic products/meat products分类
化学化工引用本文复制引用
闵宇航,刘斯琪,余晓琴,李澍才,张丽平..SPE-UPLC-MS/MS同时测定食品中24种酸性工业染料[J].食品工业科技,2024,45(1):284-294,11.基金项目
国家市场监督总局基金项目(2020-KYSB-008) （2020-KYSB-008）
四川省市场监督管理局科技计划项目(SCSJS2022005). （SCSJS2022005）
