Xu Wen, Fu Zhi-Qin, Lin Jing, Huang Xue-Cheng, Yu Hong-Min, Huang Ze-Hao, Fan Shi-Ming
Yao Xue Xue Bao. 2014 Dec;49(12):1711-7.
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 x 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 °C. 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
在本研究中，建立了一种快速灵敏的分析方法，采用超高效液相色谱-三重四极杆串联质谱联用仪（UPLC-MS/MS）的多反应监测（MRM）模式，测定了三叶崖爬藤中10种主要化合物（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）。在Waters CORTECS C18（2.1 mm×100 mm，1.6 μm）色谱柱上，以乙腈（A）和0.1%甲酸水溶液（B）为流动相，梯度洗脱，流速为0.25 mL·min⁻¹，柱温设定为45℃，进行负离子模式的UPLC-MS/MS测定。在优化的色谱条件下，10种目标化合物得到了良好的分离，包括手性异构体原花青素B1和B2在8.5 min内完全分离。线性范围宽，测定系数良好（r＞0.996 6），回收率在95.44% - 110.40%之间，相对标准偏差（RSD）在2.37% - 8.69%之间。这是首次报道采用UPLC-MS/MS法同时分析三叶崖爬藤中10种主要黄酮类成分，可以为三叶崖爬藤的质量控制提供高灵敏度、高特异性、快速高效的方法。
