摘要
采用高效液相色谱-四极杆飞行时间串联质谱(HPLC-Q-TOF MS)技术对苦杏仁与桃仁甲醇提取物中的化学成分进行鉴定,同时利用化学模式识别方法分析了2种中药的差异成分。采用Agilent SB-C18(150 mm×3.0 mm,2.7μm)色谱柱分离,以乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,质谱采用电喷雾离子源,在正、负离子模式下采集数据。对色谱图中各色谱峰进行精确质量数识别,结合数据库及二级质谱裂解规律对化学成分进行定性分析。利用Profinder软件进行预处理,结合SIMCA-P软件,建立了主成分分析(PCA)与正交偏最小二乘法判别分析(OPLS-DA)统计模型,进行差异性成分分析。苦杏仁与桃仁中共鉴定得到29个共有化学成分,其中苦杏仁苷、野黑樱苷、扁桃酸酰胺-β-龙胆二糖苷、扁桃酸-β-龙胆二糖苷、扁桃酸-β-D-吡喃葡萄糖苷和苄基-β-龙胆二糖苷等糖苷类化合物是苦杏仁与桃仁主要的难挥发化学成分。其中,15个化学成分在苦杏仁与桃仁中存在显著差异,主要包括糖苷类、氨基酸类与脂肪酸类等3类化合物。丙基-β-龙胆二糖苷在苦杏仁与桃仁中差异明显,可作为区分苦杏仁与桃仁潜在的化学标志物。该研究为苦杏仁与桃仁的药效研究及质量控制提供了数据支持。
A high-performance liquid chromatography-quadrupole time-of-flight mass spectrometric(HPLC-Q-TOF MS)method was established for the identification on constituents in Armeniacae Amarum Semen and Persicae Semen.Meanwhile,the chemical constitutions difference between Armeniacae Amarum Semen and Persicae Semen were analyzed by chemical pattern recognition methods.The sample was firstly extracted with methanol,then separated on an Agilent SB-C18 column(150 mm×3.0 mm,2.7μm)by gradient elution,with 0.1%formic acid water-acetonitrile as the mobile phase,and finally analyzed by MS in positive and negative modes.The qualitative analysis of chemical compositions was proceeded by online database,Agilent TCM PCDL database and fragmentation regularities of mass spectra,which were compared with those of standard samples.A total of 29 constituents were identified,including 8 glycoside compounds,6 amine acids,9 organic acids and 6 other compounds,in which glycoside compounds such as amygdaloside,prunasin,mandelic acid amide-β-gentiobioside,benzyl-β-gentiobioside,etc.were the main non-volatility constituents in Armeniacae Amarum Semen and Persicae Semen.Propyl-β-gentiobioside was firstly reported in these two traditional Chinese medicines.The mass data were pretreated with Profinder software.Combined with SIMCA-P software,a statistical model for the discrimination of constituents difference between these two medicines was established by unsupervised principal component analysis(PCA)and supervised orthogonal partial-least squares discriminant analysis(OPLS-DA)multivariate pattern recognition techniques.A clear distinction between Armeniacae Amarum Semen and Persicae Semen was presented when PCA and OPLS-DA were used.15 compounds showed significant differences between these two medicinal materials,which were mainly composed of glycosides,amine acids and fatty acids.Importantly,the content of propyl-β-gentiobioside in Armeniacae Amarum Semen outclassed that in Persicae Semen,which may be used as the potential chemical marker to
作者
周熙
谢斌
黄晓兰
罗辉泰
黄芳
谢梦婷
吴惠勤
ZHOU Xi;XIE Bin;HUANG Xiao-lan;LUO Hui-tai;HUANG Fang;XIE Meng-ting;WU Hui-qin(Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine,Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals,Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,Guangzhou),Guangzhou 510070,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2021年第6期940-946,共7页
Journal of Instrumental Analysis
基金
广东省科学院测试分析研究所(中国广州分析测试中心)项目(202006)。
关键词
苦杏仁
桃仁
高效液相色谱-四极杆飞行时间串联质谱
化学标志物
质量控制
Armeniacae Amarum Semen
Persicae Semen
high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry
chemical marker
quality control
