超高效液相色谱-串联四极杆-线性加速离子阱复合质谱法对加工肉制品中防腐剂、甜味剂的筛查检测

Determination of preservatives and sweeteners in processed meat by ultra performance liquid chromatography-tandem quadrupole-linear accelerated ion trap mass spectrometry

目的建立加工肉制品中5种防腐剂、6种甜味剂同时定性、定量检测的超高效液相色谱-串联质谱方法。方法样品经50%甲醇溶液提取,正己烷净化,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,多反应监测(MRM)→信息相关采集(IDA)→增强子离子扫描(EPI)模式检测。结果应用超高效液相色谱-串联四极杆-线性加速离子阱复合质谱特有的MRM-IDAEPI扫描模式,可同时实现5种防腐剂、6种甜味剂的准确定性、定量分析。经方法学验证,相关系数均>0.992,回收率为85.2%~96.7%,相对标准偏差为1.2%~12.5%,本方法的线性关系、回收率、精密度均符合要求。结论本方法应用Qtrap质谱的筛查功能,可对化合物进行进一步确证分析,避免假阳性样品的检出。

Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS/MS）method for the determination of 5 preservatives and 6 sweeteners in processed meat. Methods The samples were extracted with50% methanol solution. Extraction liquid was purified by Hexane removal. The separation of 5 preservatives and 6 sweeteners were separated on Waters Acquity UPLC system with a BEH C18 column. The mobile phases were methanol and 0. 02 mol/L ammonium acetate in gradient elution. The electrospray was operated in the negative ionization mode,and the compounds were identified by MRM→IDA→EPI scan mode. Results The MRM-IDA-EPI scanning mode of ultra performance liquid chromatography-tandem quadrupole-linear accelerated ion trap mass spectrometry could realize accurate qualitative and quantitative analysis of 5 preservatives and 6 sweeteners. The correlation coefficient was 〉0. 992,the recovery rate was within85. 2%-96. 7%,the relative standard deviation was 1. 2%-12. 5%,and the linear relationship,recovery rate and precision meet the requirements. Conclusion The method can be used to confirm the analysis of compounds by Qtrap mass spectrometry,and the detection of false positive samples can be avoided.