Fast simultaneous analysis of caffeine, trigonelline, nicotinic acid and sucrose in coffee by liquid chromatography-mass spectrometry
Fast simultaneous analysis of caffeine, trigonelline, nicotinic acid and sucrose in coffee by liquid chromatography-mass spectrometry
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DOI：
10.1016/j.foodchem.2008.03.012
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发表时间：
2008-10-15
期刊：
影响因子：
8.8
通讯作者：
Farah, Adriana
中科院分区：
文献类型：
--
作者：
Perrone, Daniel;Donangelo, Carmen Marino;Farah, Adriana
建立了同时测定咖啡中咖啡因、胡芦巴碱、烟酸和蔗糖的高效液相色谱-质谱法。该方法用热水提取，碱性醋酸铅澄清，膜过滤，Sphisorbo(R)S5 ODS2色谱柱，5µm色谱柱，0.3%甲酸/甲醇梯度洗脱，流速0.2mL/min。电喷雾电离源在负模式下工作以产生蔗糖离子，在正模式下工作以产生咖啡因、胡芦巴碱和烟酸离子。由于基质效应，所有分析物的电离均受到抑制。在绿色和烘焙咖啡提取物中制备的校准曲线与r(2)>；0.999呈线性关系。添加烘焙咖啡，咖啡因的回收率为93.0%~105.1%，胡芦巴碱为85.2%~116.2%，烟酸为89.6%~113.5%，蔗糖为94.1%~109.7%。矩阵中所有分析物的重复性良好(RSD<；5%)。咖啡因、胡芦巴碱、烟酸和蔗糖的检出限分别为11.9、36.4、18.5和5.0 ng/mL。对11个咖啡样品(普通咖啡或无咖啡因绿色咖啡、研磨烘焙咖啡和速溶咖啡)的分析结果与文献一致。该方法适用于市场上不同类型的咖啡，是一种快速、可靠的替代方法，可用于常规咖啡分析。(C)2008爱思唯尔有限公司。保留所有权利。
A rapid liquid chromatography-mass spectrometry method for the simultaneous quantification of caffeine, trigonelline, nicotinic acid and sucrose in coffee was developed and validated. The method involved extraction with hot water, clarification with basic lead acetate and membrane filtration, followed by chromatographic separation using a Spherisorbo (R) S5 ODS2, 5 mu m chromatographic column and gradient elution with 0.3% aqueous formic acid/methanol at a flow rate of 0.2 mL/min. The electrospray ionization source was operated in the negative mode to generate sucrose ions and in the positive mode to generate caffeine, trigonelline and nicotinic acid ions. Ionization suppression of all analytes was found due to matrix effect. Calibrations curves prepared in green and roasted coffee extracts were linear with r(2) > 0.999. Roasted coffee was spiked and recoveries ranged from 93.0% to 105.1% for caffeine, from 85.2% to 116.2% for trigonelline, from 89.6% to 113.5% for nicotinic acid and from 94.1% to 109.7% for sucrose. Good repeatibilities (RSD < 5%) were found for all analytes in the matrix. The limit of detection (LOD), calculated on the basis of signal-to-noise ratios of 3: 1, was 11.9, 36.4, 18.5 and 5.0 ng/mL for caffeine, trigonelline, nicotinic acid and sucrose, respectively. Analysis of 11 coffee samples (regular or decaffeinated green, ground roasted and instant) gave results in agreement with the literature. The method showed to be suitable for different types of coffee available in the market thus appearing as a fast and reliable alternative method to be used for routine coffee analysis. (C) 2008 Elsevier Ltd. All rights reserved.