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本研究建立了一种超高效液相-串联四极杆质谱多反应监测模式法同时定量6种诃子酚类有效成分:诃黎勒酸(chebulagic acid),五没食子酰葡萄糖(pentagalloyl glucose),木麻黄鞣宁(casua-rinin),鞣料云实素(corilagin),鞣花酸(ellagic acid)和没食子酸(gallic acid),选用半合成的酚类化合物4β-(L-乙酰半胱氨酸)-表儿茶素为内标。药材粉碎后用含内标的甲醇溶液超声提取,提取液用安捷伦ZORBAXEclipseX DB-C18(2.1×50mm,1.8建立方法对诃子μm)分析柱分离,甲醇-0.1%甲酸梯度洗脱,电喷雾电离源多反应模式监测。所6种成分的定量限均小于0.0868相关系数均大于μg·mL~(-1),在定量范围内成分与内标的峰面积比与成分质量浓度呈线性关系,0.99;方法回收率为83.4-108.1%;日内及日间精密度RSD分别为0.9-5.9和1.3-4.8。检测结果表明诃子果肉及种皮中这6种有效成分含量均高,以果肉中的含量最高,该法也可用于诃子及其复方的质量控制。
In this study, an ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry (MALDI-TOF MS) multi-reaction monitoring method was established for the simultaneous determination of six compounds of phenanthroline (chebulagic acid, pentagalloyl glucose, Casua-rinin, corilagin, ellagic acid and gallic acid, and the semi-synthetic phenolic compound 4β- (L-acetylcysteine Acid) - epicatechin as an internal standard. The herbs were pulverized and then extracted with methanol containing internal standard solution. The extracts were separated by analytical column with Agilent ZORBAXEclipseX DB-C18 (2.1 × 50mm, 1.8 μm), methanol-0.1% formic acid gradient elution, electrospray ionization Multiple reaction mode monitoring. The correlation coefficients between the six components were less than 0.0868 and the correlation coefficients were all greater than μg · mL -1. The linear relationship between the peak area ratio of components and internal standard and the mass concentration of components was 0.99 in the quantitative range. The recovery was 83.4% 108.1%. The intra-day and inter-day RSD were 0.9-5.9 and 1.3-4.8, respectively. The test results show that the myrobalan fruit and seed coat of these six active ingredients are high, the highest content in the flesh, the method can also be used Myrobalan and its compound quality control.