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通过优化色谱分离条件和质谱条件,建立了基于高效液相色谱-串联质谱测定赣南脐橙幼果中酚酸的测定方法。以咖啡酸、对香豆酸、阿魏酸、芥子酸、没食子酸和对羟基苯甲酸6种酚酸化合物标准品,对赣南脐橙幼果6种酚酸进行定量分析。色谱柱为Agilent-C_(18) column(2.1mm×100 mm,1.8μm),流动相为0.1%甲酸水溶液(A)/乙腈(B)进行梯度洗脱,柱温35℃,流速0.3 m L/min;质谱以负离子模式进行多反应监测模式(MRM)扫描。结果表明:利用该方法可同时对赣南脐橙幼果中的咖啡酸、对香豆酸、阿魏酸、芥子酸、没食子酸和对羟基苯甲酸6种酚酸进行定量分析;采用外标法建立了6种酚酸的定量方法,6种酚酸的标准物质在各自质量浓度范围内具有良好线性关系,相关系数为0.991~0.999,检出限为(0.04~8.92)μg/g,平均回收率为85.5%~103.9%,相对标准偏差(RSD)小于2.8%。该方法简便、快速、准确,不仅适合脐橙中酚酸化合物的含量测定,而且对于其他柑橘属植物中酚酸化合物含量的测定也具有一定参考价值。
By optimizing chromatographic conditions and mass spectrometry conditions, a method for the determination of phenolic acids in Gannan navel orange based on high performance liquid chromatography-tandem mass spectrometry was established. Six kinds of phenolic acids in young fruits of Gannan navel orange were quantitatively analyzed with six phenolic compounds as caffeic acid, p-coumaric acid, ferulic acid, erucic acid, gallic acid and p-hydroxybenzoic acid. The column was eluted with a gradient of Agilent-C 18 column (2.1 mm × 100 mm, 1.8 μm) and a mobile phase of 0.1% formic acid in water (A) / acetonitrile (B) / min; mass spectrometry Multiple reaction monitoring mode (MRM) scanning in negative ion mode. The results showed that the six phenolic acids of cauliflower, p-coumaric acid, ferulic acid, erucic acid, gallic acid and p-hydroxybenzoic acid in Gannan navel orange fruit could be quantitatively analyzed by this method. Six kinds of phenolic acids were established. The calibration curves of six kinds of phenolic acids were linear in the range of their respective mass concentrations. The correlation coefficients were 0.991-0.999. The detection limits were (0.04-9.92) μg / g. The average recoveries Rates ranged from 85.5% to 103.9% with relative standard deviations (RSDs) less than 2.8%. The method is simple, rapid and accurate. It is not only suitable for the determination of phenolic compounds in navel orange, but also has certain reference value for the determination of phenolic compounds in other citrus plants.