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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 a method for the simultaneous qualitative and quantitative determination of 5 kinds of preservatives and 6 kinds of sweeteners in processed meat products by ultra performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with 50% methanol and purified with n-hexane. The sample was separated on a Waters Acquity UPLC BEH C18 column and eluted with methanol and 0.02 mol / L ammonium acetate as mobile phase. The electrospray negative ion (ESI-) , Multiple reaction monitoring (MRM) → information-dependent acquisition (IDA) → enhanced ion scan (EPI) mode. Results The MRM-IDAEPI scanning mode, which is unique to the ultra performance liquid chromatography-tandem quadrupole-linear accelerator ion trap mass spectrometry, was used to achieve accurate qualitative and quantitative analysis of five preservatives and six sweeteners simultaneously. The methodological validation showed that the correlation coefficient was> 0.992, the recoveries were 85.2% ~ 96.7% and the relative standard deviations were 1.2% ~ 12.5%. The linear relationship, recovery and precision of this method all met the requirements. Conclusion The method of Qtrap MS screening can be used to further confirm the compounds to avoid false positive samples.