Quantitative thin-layer chromatography/mass spectrometry analysis of caffeine using a surface sampling probe electrospray ionization tandem mass spectrometry system

被引:51
作者
Ford, MJ [1 ]
Deibel, MA [1 ]
Tomkins, BA [1 ]
Van Berkel, GJ [1 ]
机构
[1] Oak Ridge Natl Lab, Organ & Biol Mass Spectrometry Grp, Div Chem Sci, Oak Ridge, TN 37831 USA
关键词
D O I
10.1021/ac050488s
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
Quantitative determination of caffeine on reversed-phase CS thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 mu m/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methods determined from the calibration curve statistics were 0.20 ng injected (0.50 mu L) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by similar to 8% or more) than the literature values.
引用
收藏
页码:4385 / 4389
页数:5
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