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
闵宇航 1刘斯琪 1余晓琴 1李澍才 1张丽平2
作者信息
- 1. 四川省食品检验研究院,四川成都 611731;国家市场监管重点实验室(白酒监管技术),四川成都 611731
- 2. 成都纺织高等专科学校轻工与材料学院,四川成都 611731
- 折叠
摘要
建立了固相萃取-超高效液相色谱串联质谱法同时测定食品中 24种酸性工业染料的分析方法.样品经氨水乙醇溶液(氨水:无水乙醇:水=2:7:1,v/v/v)提取,提取液氮吹浓缩至 1 mL,加入 10 mL 5%甲醇水溶液,弱阴离子交换固相萃取柱(Agela Cleanert PWAX)富集净化,氮吹复溶后,Agilent ZORBAX Eclipse RRHD C18(3.0 mm×150 mm,1.8 μm)色谱柱分离,流动相采用乙腈和 10 mmol/L乙酸铵溶液进行梯度洗脱,电喷雾离子源负离子进行电离,多反应监测模式(MRM)下测定,外标法定量.结果表明,24种酸性工业染料在 20～300 ng/mL范围内,相关系数r均大于 0.999;方法检出限为 10 μg/kg,定量限为 25 μg/kg;在 25、100、250 μg/kg三个不同加标水平下的回收率为 91.0%～112.7%,相对标准偏差(n=6)为 0.42%～4.39%.采用该方法对市售的豆制品、调味品、水产品、肉制品各 40批次进行测定,2批次卤肉样品中检出酸性橙Ⅱ,含量分别为 138±2.8 μg/kg和 179±3.7 μg/kg;2批次香肠样品中检出红 2G,含量分别为 320±8.6 μg/kg和 230±6.2 μg/kg.该方法灵敏、快速、准确,适用于食品中24种酸性工业染料的定性定量测定.
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引用本文复制引用
基金项目
国家市场监督总局基金(2020-KYSB-008)
四川省市场监督管理局科技计划项目(SCSJS2022005)
出版年
2024
国家科技期刊平台
NSTL
维普
万方数据