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作 者:蔡琼 余文琴 李小琴 阮燕 李姗 史沁芳 程龙 CAI Qiong;YU Wen-Qin;LI Xiao-Qin;RUAN Yan;LI Shan;SHI Qin-Fang;CHENG Long(Chongqing Academy of Metrology and Quality Inspection,Chongqing 401121,China;SCIEX,Shanghai 200335,China)
机构地区:[1]重庆市计量质量检测研究院,重庆401121 [2]上海爱博才思分析仪器贸易有限公司,上海200335
出 处:《食品安全质量检测学报》2024年第4期87-97,共11页Journal of Food Safety and Quality
基 金:重庆市计量质量检验研究院科研计划项目(2022研-14、2022研-15)。
摘 要:目的基于高效液相色谱-三重四极杆/复合线性离子阱质谱法(high performance liquid chromatography-triple quadrupole/composite linear ion trap mass spectrometry,HPLC-QTRAP MS)建立同时测定液态发酵食品中14中生物胺及其代谢物的分析方法。方法采用Waters Atlantis Premier BEH Z-HILIC色谱柱(100mm×2.1mm,1.7μm),以0.025%(V/V)甲酸水和0.1%(V/V)甲酸乙腈进行梯度洗脱,电喷雾离子源(electrospray ionization,ESI)正离子模式、多反应监测(multiple reaction monitoring,MRM)离子扫描模式、信息依赖性采集(information dependent acquisition,IDA)、增强子离子扫描(enhanced ion scanning,EPI)和EPI谱库搜索的复合模式进行测定。结果在0.05~200.00μg/L质量浓度范围内,14种生物胺及其代谢物的线性关系良好,相关系数均大于0.99;方法检出限(S/N=3)为0.15~6.00μg/L;在不同添加质量浓度(2.0、10.0、50.0μg/L)下,其回收率为75.2%~107.9%,相对标准偏差在1.98%~9.07%之间。结论该方法具有操作简便、快速、准确、灵敏等优点,可满足液态类发酵食品中14种生物胺的定性定量分析需要,为液态发酵类食品中生物胺的检测分析奠定基础。Objective To establish a method for the simultaneous determination of 14 kinds of biogenic amines and their metabolites in liquid fermented food by high performance liquid chromatography-triple quadrupole/composite linear ion trap mass spectrometry(HPLC-QTRAP MS).Methods Using 0.025%(VIV)formic acid/water solution and 0.1%(V/V)formic acid/acetonitrile as mobile phase,the mixture was separated on Waters Atlantis Premier BEH Z-HILIC Column(100 mm×2.1 mm,1.7μm).The target compounds were analyzed using electrospray ionization(ESI)positive ion mode,multiple reaction monitoring(MRM),information dependent acquisition(IDA),enhanced ion scanning(EPI),and multi-step mode analysis combined with EPI library retrieval of 14 kinds of biogenic amines and their metabolites.Results The results showed that the linearity of 14 kinds of biogenic amines and their metabolites were pretty good when the mass concentration was from 0.05-200.00μg/L.The correlation coefficients were all above 0.99.The limits of detection(S/N=3)were 0.15-6.00μg/L.The mean recoveries at 2.0,10.0,50.0μg/L were 75.2%-107.9%and the relative standard deviations were 1.98%-9.07%.Conclusion The established method is convenient to operate,has short analysis time,high accuracy and sensitivity,which can meet the qualitative and quantitative needs of 14 kinds of biogenic amines in liquid fermented food,and provide strong technical support for the detection of biogenic amines in liquid fermented food.
关 键 词:生物胺 代谢产物 高效液相色谱-三重四极杆/复合线性离子阱质谱法 液态发酵食品
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