摘要
建立了肉制品中6种甜味剂检测的超高效液相色谱-串联质谱分析方法。利用Qtrap质谱特有的EPI扫描模式对化合物进行鉴定,并通过谱库检索对化合物进行确证。样品经50%甲醇溶液提取,提取液经正己烷净化,6种甜味剂经Waters Acquity UPLC BEH C18色谱柱分离,以甲醇和0.02 mol/L乙酸铵水溶液为流动相进行梯度洗脱。电喷雾负离子(ESI-)模式电离,MRM→IDA→EPI扫描模式检测,外标法定量。结果表明:6种甜味剂在0.01~2.0μg/m L范围内呈良好的线性关系,相关系数(r)均大于0.99;香肠中3个浓度添加水平平均回收率为81.3%~95.6%;相对标准偏差为2.25%~9.86%。该方法具有操作简便、灵敏度高、定性准确等特点。
An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the determination of 6 sweetener in processed meats. And a new Qtrap system was used to identify the compound with EPI scan mode, and Identification of the purity of the compound with data library. Samples were extracted with 50% methanol solution. Extraction liquid was purified by n-hexane. The separation of 6 sweetener were performed on a Waters Acquity UPLC system with a BEH C18 column. The mobile phases were methanol and 0.02 mol/L anunonium acetatein gradient elution. The electrospray was operated in the negative ionization mode and the 6 sweetener were identified by MRM → IDA → EPI scan mode, quantitatived by external standard method. The calibration curves showed good linearity within the concentrations of 0.01 - 2.0μ g/mL with the correlation coefficients r 〉 0.99. The recoveries of 6 sweetener were 81.3% - 95.6% at the spiked levels of 0.05, 0.1, 0.5 mg/ kg. The relative standard deviations coefficients of variation were both less than 2.25% - 9.86%. This method is simple, sensitive and accurate in the determination of sweetener.
出处
《中国食品添加剂》
CAS
北大核心
2016年第10期194-197,共4页
China Food Additives
基金
辽宁出入境检验检疫局科技计划项目(LK18-2015)