基于UPLC-Q-TOF-MS和HPLC的不同品种白芍主要化学成分分析  

Analysis and evaluation on Paeoniae Radix Alba from different cultivars by UPLC-Q-TOF-MS and HPLC

作　　者：杨爽 杜倩倩 岳倩侠 孙叶芬 金传山[1,2] 张伟 马磊[3] 刘丛彬 谢冬梅[1,2] YANG Shuang;DU Qian-qian;YUE Qian-xia;SUN Ye-fen;JIN Chuan-shan;ZHANG Wei;MA Lei;LIU Cong-bin;XIE Dong-mei(Anhui University of Chinese Medicine,Hefei 230012,China;Institute of Chinese Medicine Resources Protection and Development,Anhui Academy of Traditional Chinese Medicine,Hefei 230012,China;Anhui Jiren Pharmaceutical Co.,Ltd.,Bozhou 236800,China)

机构地区：[1]安徽中医药大学,安徽合肥230012 [2]安徽省中医药研究院中药资源保护与开发研究所,安徽合肥230012 [3]安徽济人药业股份有限公司,安徽亳州236800

出　　处：《中国中药杂志》2023年第3期715-724,共10页China Journal of Chinese Materia Medica

基　　金：亳州市科技重大专项(bzzd2020002);2019年全国中药特色技术人才培训项目(T2-194828003);安徽省重点研究与开发计划项目(202104h04020029)。

摘　　要：应用超高液相色谱-串联四极杆飞行时间质谱(UPLC-Q-TOF-MS)技术结合多元统计分析药材白芍的不同栽培品种的药用部位中主要化学成分的异同性;建立高效液相色谱法(HPLC)同时测定白芍中8种活性成分的方法。UPLC-Q-TOF-MS采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),柱温30℃,0.1%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱,流速0.2 mL·min^(-1);电喷雾离子源,正、负离子模式下采集质谱数据,其中正、负离子模式下鉴定了不同栽培品种白芍根中的36种主要相同成分,负离子模式筛选并鉴定了17种含量显著性差异成分,1种“亳白芍”中特有成分。采用HPLC进行定量分析,使用Agilent HC-C18色谱柱(4.6 mm×250 mm,5μm),柱温30℃,0.1%磷酸水溶液(A)-乙腈(B)为流动相,梯度洗脱,流速1.0 mL·min^(-1),检测波长230 nm,建立了HPLC同时测定白芍根中8种活性成分(没食子酸、氧化芍药苷、儿茶素、芍药内酯苷、芍药苷、没食子酰芍药苷、1,2,3,4,6-O-五没食子酰葡萄糖、苯甲酰芍药苷)的含量测定方法,各成分的线性关系良好(r>0.9990),精密度、重复性和稳定性良好,平均回收率为90.61%~101.7%,RSD为0.12%~3.6%(n=6)。UPLC-Q-TOF-MS为鉴定白芍的化学成分提供了一种快速、高效的定性分析方法;所建立的HPLC同时测定8个活性成分含量的方法简便、快捷、准确,为不同栽培品种白芍的种质资源和药材质量评价提供了科学依据。In this study, an established ultra-high performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry(UPLC-Q-TOF-MS) method was combined with multivariate statistical analysis to investigate the commonality and difference of main chemical components in the medicinal parts of Paeonia lactiflora from different cultivars;in addition, a high performance liquid chromatography(HPLC) method was established to simultaneously determine the content of eight active components in Paeoniae Radix Alba. Non-targeted analysis was carried out by UPLC-Q-TOF-MS on a Waters ACQUITY UPLC BEH C18(2.1 mm×100 mm, 1.7 μm) column with a gradient elution of 0.1% aqueous formic acid(A)-acetonitrile(B) as the mobile phase at a flow rate of 0.2 mL·min^(-1). The column temperature was 30 ℃, and an electrospray ionization source was used to acquire mass spectrometry data in positive and negative ion modes. According to the accurate molecular weight and fragment ion information provided by multi-stage mass spectrometry and by comparison with reference substances and literature reports, thirty-six identical components were identified in Paeoniae Radix Alba from different cultivars with positive and negative ion modes. In the negative ion mode, two groups of samples were well separated;specifically, seventeen components with significant differences in content were screened and identified, and one component unique in "Bobaishao" was obtained. Quantitative analysis was conducted by high-performance liquid chromatography(HPLC) on an Agilent HC-C18(4.6 mm×250 mm, 5 μm) column with a gradient elution of 0.1% aqueous phosphoric acid(A)-acetonitrile(B) as the mobile phase at a flow rate of 1.0 mL·min^(-1). The column temperature was 30 ℃ and the detection wavelength was at 230 nm. An HPLC method was developed for the simultaneous determination of eight active components(gallic acid, oxypaeoniflorin, catechin, albiflorin, paeoniflorin, galloylpaeoniflorin, 1,2,3,4,6-O-pentagalloylglucose, benzoyl-paeoniflorin) in Pa

关 键 词：白芍 品种 UPLC-Q-TOF-MS HPLC 质量评价 

分 类 号：R284.1[医药卫生—中药学] O657[医药卫生—中医学]