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

作　　者：闵宇航 刘斯琪 余晓琴 李澍才 张丽平[3] MIN Yuhang;LIU Siqi;YU Xiaoqin;LI Shucai;ZHANG Liping(Sichuan Institute of Food Inspection,Chengdu 611731,China;Key Laboratory of Baijiu Supervising Technology for State Market Regulation,Chengdu 611731,China;Department of Light Industry and Materials,Chengdu Textile College,Chengdu 611731,China)

机构地区：[1]四川省食品检验研究院,四川成都611731 [2]国家市场监管重点实验室(白酒监管技术),四川成都611731 [3]成都纺织高等专科学校轻工与材料学院,四川成都611731

出　　处：《食品工业科技》2024年第1期284-294,共11页Science and Technology of Food Industry

基　　金：国家市场监督总局基金项目(2020-KYSB-008);四川省市场监督管理局科技计划项目(SCSJS2022005)。

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 C_(18)(3.0 mm×150 mm,1.8μm)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10μg/kg,定量限为25μg/kg;在25、100、250μg/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±2.8μg/kg和179±3.7μg/kg;2批次香肠样品中检出红2G,含量分别为320±8.6μg/kg和230±6.2μg/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。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 C_(18)(3.0 mm×150 mm,1.8μm)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 10μg/kg and 25μg/kg.The recoveries at three level spiked levels(25、100、250μg/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 orangeⅡwas detected in 2 batches of braised meat samples,the content was 138±2.8μg/kg and 179±3.7μg/kg,the red 2G was detected in 2 batches of sausage samples,the content was 320±8.6μg/kg and 230±6.2μg/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 

分 类 号：O657.63[理学—分析化学]