Jin Hua, Tang Ge, Li Jin, Ma Lin, Li Yuhong, Chang Yan-Xu
College of Traditional Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China.
Department of Nephrology, The First Teaching Hospital of Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China.
J Anal Methods Chem. 2020 Aug 26;2020:8861765. doi: 10.1155/2020/8861765. eCollection 2020.
A sensitive and accurate method was developed for the simultaneous determination of twelve components including phenolic acids (gallic acid, protocatechuic aldehyde, protocatechuic acid, and ferulic acid), flavonoids (catechin, epicatechin, rutin, luteolin, luteolin-7-glucoside, and epicatechin gallate), anthraquinones (emodin), and triterpenes (ursolic acid) in Cynomorii herba in different harvest times by liquid chromatography tandem mass spectrometry (LC-MS/MS). The chromatographic separation was achieved on an Eclipse plus C (3.0 mm × 50 mm, 1.8 m) column at 40°C. The mobile phase consisted of acetonitrile and 0.05% formic acid with a gradient elution at a flow rate of 0.4 mL·min . Under the optimized conditions, there was good linear relation ( ≥ 0.9944) and satisfactory precision (RSD values less than 5.65%). The recoveries of the twelve components were in the range of 93.5-105%. Moreover, the limits of detection (LOD) ranged from 0.003 to 21 ng mL for the twelve analytes. In conclusion, the validated method was successfully applied to analyze the change regularity of the twelve components of Cynomorii herba in different harvest times. It provides a theoretical basis for choosing the suitable harvesting time of Cynomorii herba.
建立了一种灵敏、准确的方法，采用液相色谱串联质谱法（LC-MS/MS）同时测定锁阳在不同采收期的12种成分，包括酚酸类（没食子酸、原儿茶醛、原儿茶酸和阿魏酸）、黄酮类（儿茶素、表儿茶素、芦丁、木犀草素、木犀草素-7-葡萄糖苷和表儿茶素没食子酸酯）、蒽醌类（大黄素）和三萜类（熊果酸）。色谱分离在Eclipse plus C（3.0 mm×50 mm，1.8 μm）柱上于40°C下进行。流动相由乙腈和0.05%甲酸组成，采用梯度洗脱，流速为0.4 mL·min 。在优化条件下，线性关系良好（r≥0.9944），精密度令人满意（RSD值小于5.65%）。12种成分的回收率在93.5%至105%之间。此外，12种分析物的检测限范围为0.003至21 ng mL 。总之，该验证方法成功应用于分析锁阳在不同采收期12种成分的变化规律。为选择锁阳合适的采收时间提供了理论依据。
