高效液相色谱-串联质谱法同时测定山楂中6个黄酮类功效成分

目的：建立山楂中6个黄酮类物质的液相色谱-串联质谱（LC-MS/MS）测定方法。方法：实验优化了液相色谱条件和质谱参数。采用C₁₈柱分离，流动相为乙腈-水（含0.1%甲酸），梯度洗脱，流速0.2 mL·min^-1，以电喷雾离子源正离子多反应监测（MRM）模式进行MS/MS检测。结果：6个黄酮类物质在各自的线性范围内具有良好的线性关系，相关系数大于0.994，低、中、高3个添加水平的平均回收率在80.4%~105.0%之间，RSD小于10%。10批样品中6个黄酮成分的含量测定结果：儿茶素，0.03~5.39 μg·g^-1；牡荆素，0.11~1.02 μg·g^-1；木犀草素，0.02~0.09 μg·g^-1；槲皮素，3.72~14.02 μg·g^-1；芦丁，3.32~5.79 μg·g^-1；金丝桃苷，31.32~80.89 μg·g^-1。结论：该方法可用于测定山楂中儿茶素、牡荆素、槲皮素、木犀草素、芦丁、金丝桃苷。

Objective:To establish a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method for simultaneous determination of 6 functional components in hawthorn. Methods:The conditions of chromatography and mass spectrometry were optimized. The 6 flavonoids were separated on a C₁₈ chromatographic column with acetonitrile and 0.1% formic acid as mobile phase under gradient elution at a flow rate of 0.2 mL·min^-1. The determination was conducted by tandem mass spectrometry in positive ESI mode under multiple reaction monitoring(MRM) mode. Results:Good linearities for all the compounds,with correlation coefficients over 0.994,were acquired. The recoveries(n=6) were in the range of 80.4% to 105.0%,while RSDs were less than 10%. The contents of 6 functional components in 10 batches of samples were as follows:catechin,0.03-5.39 μg·g^-1;vitexin,0.11-1.02 μg·g^-1;luteolin,0.02-0.09 μg·g^-1;quercetin,3.72-14.02 μg·g^-1;rutin,3.32-5.79 μg·g^-1;hyperoside,31.32-80.89 μg·g^-1. Conclusion:The established method can be used to determine catechin,vitexin,quercetin,luteolin,rutin and hyperoside in hawthorn.