摘要
目的建立高效液相色谱-串联质谱法同时检测饮料中多种添加剂的分析方法.方法称取样品直接加入50%甲醇溶液,涡旋振荡提取5 min后经聚四氟乙烯(polytetrafluoroethylene,PTFE)滤膜过滤,滤液直接上机进行检测.本实验采用Atlantis T3色谱柱(2.1 mm×150 mm,3μm),10 mmol/L乙酸铵-乙腈作为流动相体系进行梯度洗脱;在电喷雾离子化(ESI)正负离子扫描模式下,以多重反应监测(multiple reaction monitoring,MRM)为基础进行检测,通过外标法进行定量分析;最后,考察了不同浓度的溶剂对目标分析物的提取效率及不同规格的滤膜对目标分析物的吸附效应.结果此方法可快速准确检测苯甲酸等16种食品添加剂,浓度范围在0.02~1μg/mL内线性相关良好,相关系数(r)均大于0.995,平均回收率为75.92%~114.13%,相对标准偏差(relative standard deviation,RSD)为0.42%~7.69%(n=6).结论本方法适用于同时快速检测饮料中的多种添加剂.
Objective To establish a method for the simultaneous determination of various additives in beverages by high performance liquid chromatography-tandem mass spectrometry.Methods After adding 50%methanol liquid,the sample was extracted by vortex oscillation for 5min and then filtered by PTFE filter membrane.The filtrate was directly put on the machine for detection.Atlantis T3 column(2.1 mm×150 mm,3 mum)was used as chromatographic column and 10 mmol/L ammonium acetate-acetonitrile was used as mobile phase system for gradient elution.Under the electrospray ionization(ESI)mode with positive and negative ions,multiple reactions monitoring(MRM)was used as the basis for quantitative analysis by external standard method.The dissolution and adsorption effects of different concentrations of solvent and different sizes of filter membrane on the target analyte were optimized.Results This method could quickly and accurately detect 16 kinds of food additives,such as benzoic acid.The 16 kinds of food additives had good linear relationships in the range of 0.02-1μg/mL,and the correlation coefficients(r)were all more than 0.995.The average recoveries were 75.92%-114.13%,with relative standard deviation(RSD)of 0.42%-7.69%(n=6).Conclusion This method is suitable for the rapid detection of a variety of additives in beverages at the same time.
作者
陈宁周
王海波
莫紫梅
覃海倩
王警
郑娟梅
CHEN Ning-Zhou;WANG Hai-Bo;MO Zi-Mei;QIN Hai-Qian;WANG Jing;ZHENG Juan-Mei(Guangxi-ASEAN Center for Food and Drug Safety Control,Nanning 530021,China;College of Pharmacy,Guangxi University of Chinese Medicine,Nanning 530200,China)
出处
《食品安全质量检测学报》
CAS
2019年第15期5137-5147,共11页
Journal of Food Safety and Quality
基金
广西-东盟食品药品安全检验检测中心2019科研项目(KY201904)~~
关键词
高效液相色谱-串联质谱法
添加剂
饮料
high performance liquid chromatography-tandem mass spectrometry
additives
beverage
