液相色谱-串联质谱法检测干制水产品中9种酸性偶氮类着色剂  

Determination of Nine Acid Azo Dyes in Dried Aquatic Products by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：颜春荣 高惠敏 林慧 徐春祥 YAN Chunrong;GAO Huimin;LIN Hui;XU Chunxiang(Jiangsu Institute for Food and Drug Control,Nanjing 210008,China)

机构地区：[1]江苏省食品药品监督检验研究院,江苏南京210008

出　　处：《食品科技》2020年第11期301-305,共5页Food Science and Technology

基　　金：南京市科委2016年公共事业科技项目(201608004)。

摘　　要：目的:通过对前处理方法和检测条件进行优化,建立干制水产品中9种酸性偶氮类着色剂的液质联用检测方法。方法:干制水产品样品经均质、脱脂,用乙醇-氨水-水(体积比7:2:1)提取酸性偶氮类着色剂,并利用聚酰胺固相萃取柱净化,最后用液相色谱-串联四级杆质谱联用仪进行分析。采用Waters Acquity UPLC RHSS-C18(2.1 mm×50 mm,1.8μm)色谱柱,用甲醇和10 mmol/L乙酸铵溶液梯度洗脱,在7 min内可以完全分离。在电喷雾负离子模式(ESI-)下,用多重反应监测(MRM)方式进行离子监测,外标法定量。结果:利用液相色谱-串联四级杆质谱联用仪进行定量检测,酸性橙Ⅱ、酸性红和酸性大红GR在0.1~100μg/L,相关系数(r2)均大于0.998,检出限和定量限分别为0.10μg/kg和0.25μg/kg,添加浓度0.25、1.0、2.5μg/kg的回收率为87.5%~94.2%,相对标准偏差为5.0%~7.8%。其余6种着色剂在1~1000μg/L,相关系数(r2)均大于0.995,检出限和定量限分别为1.0μg/kg和2.5μg/kg,添加浓度为2.5、5.0、25.0μg/kg的其余6种着色剂,回收率为78.7%~89.3%,RSD为4.0%~7.2%。结论:文章建立的方法具高回收率、高灵敏度的优点,适用于干制水产品中9种酸性偶氮类着色剂的检测。Objective:The determination of 9 acid azo dyes in dried aquatic products by ultra-performance liquid chromatography-tandem mass spectrometry was established through modifying sample preparation and analysis methods.Methods:The homogenized dried aquatic product samples were extracted by mixture of ethanol,ammonium hydroxide and water(7:2:1,v/v/v),then purified by polyamide based solid phase extraction cartridge,the extractions were analyzed using ultra-performance liquid chromatography-tandem mass spectrometry.These analysts were completely separated in 7 minutes by a Waters Acquity UPLC RHSS-C18(2.1 mm×50 mm,1.8μm)column utilizing gradient elution with methanol and 10 mmol/L ammonium acetate solution.The dyes were detected by tandem mass spectrometry in negative ESI mode and calibrated by external standards.Results:The linear range of OrangeⅡ,Brilliant Crocein and Azorubine was 0.1~100μg/L with the correlation coefficients more than 0.998,the detection limits and quantitative limits were 0.10μg/kg and 0.25μg/kg respectively,when spiked at 0.25μg/kg,1.0μg/kg and 2.5μg/kg,the recovery rates were 87.5%~94.2%with relative standard deviation(RSD)5.0%~7.8%.While the linear range of the other 6 dyes was 1~1000μg/L with the correlation coefficients more than 0.995,the limits of detection(LOD)and limits of quantification(LOQ)were 1.0μg/kg and 2.5μg/kg respectively,when spiked at 2.5,5.0μg/kg and 25μg/kg,the recovery rates were 78.7%~89.3%with RSD 5.0%~7.8%.Conclusion:With the advantages of high recovery rates and satisfied sensitivity,the method developed in this study is applicable for determination of 9 acid azo dyes in dried aquatic products.

关 键 词：干制水产品 酸性偶氮类着色剂 固相萃取 高效液相色谱-串联四级杆质谱联用仪 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]