全自动固相萃取-超高效液相色谱-串联质谱法测定果酒中14种有机酸

Determination of 14 kinds of organic acids in fruit wine by automated solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  果酒  有机酸  超高效液相色谱-串联质谱法

英文关键词:fruit wine  organic acids  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立全自动固相萃取-超高效液相色谱-串联质谱法(ultra performance liquid chromatography- tandem mss spectrometry, UPLC-MS/MS)检测果酒中14种有机酸的方法。方法 采用MAX固相萃取小柱净化, Agilent Eclipse Plus RRHD C18柱(150 mm×3.0 mm, 1.8 μm)分离, 0.4%甲酸溶液-乙腈为流动相梯度洗脱, 电喷雾离子源负离子模式下, 结合动态多反应监测模式, 外标法定量。结果 14种有机酸在各自的线性范围内相关系数均大于0.991, 方法的检出限为0.7~50.0 μg/L, 方法的定量限为2.0~150.0 μg/L, 回收率为82.6%~117.1%, 相对标准偏差为0.6%~8.7% (n=6)。结论 该方法操作简单、灵敏、重现性好, 适用于果酒中有机酸的定性定量测定。

英文摘要:

      Objective To establish an analytical method for the determination of 14 kinds of organic acids in fruit wine by automated solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were purified by MAX SPE columns. The analytes were separated on a Agilent Eclipse Plus RRHD C18 column (150 mm×3.0 mm, 1.8 μm) by gradient elution with 0.4% formic acid-acetonitrile solution as the mobile phases. The MS analysis was performed by dynamic multiple reaction monitoring mode in the negative ion mode. The external standard method was used for quantification. Results The developed method showed good linearity for 14 kinds of organic acids with the correlation coefficients (r2) greater than 0.991, the limits of detection ranged from 0.7 to 50.0 μg/L. The limits of quantification ranged from 2.0 to 150.0 μg/L. The recoveries were in the range of 82.6%–117.1% with the relative standard deviations of 0.6%–8.7% (n=6). Conclusions The method is simple, sensitive and reproducible, and is suitable for the qualitative and quantitative determination of organic acids in fruit wine.