药学学报, 2014, 49(12): 1711-1717
引用本文:
许文, 傅志勤, 林婧, 黄学城, 于虹敏, 黄泽豪, 范世明. UPLC-MS/MS法同时测定三叶青中10种黄酮类成分[J]. 药学学报, 2014, 49(12): 1711-1717.
XU Wen, FU Zhi-qin, LIN Jing, HUANG Xue-cheng, YU Hong-min, HUANG Ze-hao, FAN Shi-ming. Rapid simultaneous determination of ten major flavonoids in Tetrastigma hemsleyanum by UPLC-MS/MS[J]. Acta Pharmaceutica Sinica, 2014, 49(12): 1711-1717.

UPLC-MS/MS法同时测定三叶青中10种黄酮类成分
许文1,2,3, 傅志勤1, 林婧3, 黄学城1, 于虹敏1, 黄泽豪1, 范世明1
1. 福建中医药大学, 药学院, 福建 福州 350122;
2. 福建中医药大学, 生物医药研发中心, 福建 福州 350122;
3. 福建中医药大学, 中西医结合研究院, 福建 福州 350122
摘要:
建立超高效液相色谱串联三重四级杆质谱法 (UPLC-MS/MS) 同时测定三叶青中10种黄酮类成分 (原花青素B1、儿茶素、原花青素B2、芦丁、异槲皮苷、山柰酚-3-O-芸香糖苷、紫云英苷、槲皮苷、槲皮素和山柰酚) 的含量.采用UPLC-MS/MS法及负离子多反应监测 (MRM) 模式进行含量测定.色谱条件: 色谱柱为Waters CORTECS C18 (2.1 mm × 100 mm, 1.6 μm), 流动相为乙腈 (A) - 0.1% 甲酸水 (B), 梯度洗脱, 流速0.25 mL·min-1, 柱温45 ℃.在所设定的色谱条件下, 手性异构体原花青素B1和B2达到基线分离.定量分析的三 叶青中10种黄酮类成分在考察的浓度范围内呈良好的线性关系 (r > 0.996 6); 回收率和RSD分别在95.44%~110.40% 和2.37%~8.69% 内.本研究所建立的同时测定三叶青中10种黄酮类成分的UPLC-MS/MS定量分析 方法简便、快捷、准确, 可为综合评价三叶青的质量提供参考.
关键词:    三叶青      UPLC-MS/MS      黄酮      质量控制     
Rapid simultaneous determination of ten major flavonoids in Tetrastigma hemsleyanum by UPLC-MS/MS
XU Wen1,2,3, FU Zhi-qin1, LIN Jing3, HUANG Xue-cheng1, YU Hong-min1, HUANG Ze-hao1, FAN Shi-ming1
1. School of Pharmacy, Fuzhou 350122, China;
2. Centre of Biomedical Research and Development, Fuzhou 350122, China;
3. Academy of Integrative Medicine, Fujian University of Traditional Chinese Medicine, Fuzhou 350122, China
Abstract:
In this study, a rapid and sensitive analytical method was developed for the determination of 10 major compounds (procyanidin B1, catechin, procyanidin B2, rutin, isoquercitrin, kaempferol-3-O-rutinoside, astragalin, quercitrin, quercetin, and kaempferol) in Tetrastigma hemsleyanum by using ultra-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (UPLC-MS/MS) in multiple-reaction monitoring (MRM) mode. UPLC-MS/MS assay with negative ion mode was performed on a Waters CORTECS C18 (2.1 mm × 100 mm, 1.6 μm) with the mobile phase consisting of acetonitrile (A) and 0.1% aqueous formic acid (B) in gradient elution at a flow rate of 0.25 mL·min-1 and the column temperature was set at 45 ℃. Under the optimized chromatographic conditions, good separation for 10 target compounds were obtained including chiral isomer procyanidins B1 and B2 were completely separated within 8.5 min. Satisfactory linearity was achieved with wide linear range and fine determination coefficient (r > 0.996 6), the overall recoveries were ranged from 95.44%-110.40% with the RSD ranging from 2.37%-8.69%. It is the first report about simultaneous analysis of 10 major flavonoids components in Tetrastigma hemsleyanum by using UPLC-MS/MS method, which affords highly sensitive, specific, speedy and efficient method for quality control of Tetrastigma hemsleyanum.
Key words:    Tetrastigma hemsleyanum    UPLC-MS/MS    flavonoid    quality control   
收稿日期: 2014-06-17
基金项目: 福建省教育厅资助课题(JA13154);福建中医药大学校管课题(中药学重点学科,X2013017,X2013027);福建省"大学生创新创业训练计划"项目(201410393063).
通讯作者: 黄泽豪, 范世明
Email: huangzehao@fudan.edu.cn;r3570379@163.com
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