液相色谱-串联质谱法同时测定烟草中6种Amadori化合物

Simultaneous Determination of Six Kinds of Amadori Compounds in Tobaccos by LC-MS/MS

  • 摘要: 建立了液相色谱-串联质谱法同时测定烟草中6种Amadori化合物的定性和定量分析方法。试样以70%甲醇水溶液为萃取剂,经过正交实验优化后的超声萃取条件为:料液比1∶30、萃取功率120 W,萃取时间25 min。所得萃取液用正己烷洗涤除去杂质后,在选择反应监测模式下进行液相色谱-串联质谱定性及定量分析,其中Amadori化合物采用外标标准曲线法定量。结果表明:所测定的6种Amadori化合物线性关系良好,相关系数r均大于0.995 0。方法的检出限(LOD)为20.06~39.86 μg/kg,定量限(LOQ)为66.85~132.9 μg/kg,平均回收率在86.56%~88.86%之间,相对标准偏差(RSD)均小于5%。该方法简便、灵敏度高、重现性好,适用于烟草中Amadori化合物的定性和定量分析。

     

    Abstract: A liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for qualitatively and quantitatively analyzing six kinds of Amadori compounds (Fru-Gly, Fru-Ala, Fru-Pro,Fru-Thr,Fru-Glu and Fru-Amb) in tobaccos was developed. The sample was extracted with 70% methanol water solutionsand assisted by ultrasound, and the extraction conditions which were optimized by orthogonal experiment as followings: the solid liquid ratio was 1∶30, the extraction power was 120 W,and the extraction time was 25 min. The extraction products from tobaccos were cleaned up by hexane and then analyzed by LC-MS/MS under the selected reaction monitoring (SRM) mode. The contents of six kinds of Amadori compounds were determined by external standard curve method. The results show that the limits of detection (LOD) are 20.06-39.86 μg/kg, and limits of quantity (LOQ) are 66.85-132.9 μg/kg. The correlation coefficients are greater than 0.995 0, the average recoveries are 86.56%-88.86%, and the relative standard deviations(RSD) are less than 5%. This method is simplify, sensitive and accurate, which is suitable for qualitative and quantitative analysis of Amadori compounds in tobaccos.

     

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