目的:采用液相色谱与四极杆飞行时间质谱(UPLC-QTOF/MS)联用技术,对活血通络粉针剂中的化学成分进行定性鉴别。方法:采用Themro(3 mm×100 mm,1.7μm)色谱柱,以甲醇-0.02%甲酸为流动相,梯度洗脱,体积流量为0.4 m L·min-1,柱温...目的:采用液相色谱与四极杆飞行时间质谱(UPLC-QTOF/MS)联用技术,对活血通络粉针剂中的化学成分进行定性鉴别。方法:采用Themro(3 mm×100 mm,1.7μm)色谱柱,以甲醇-0.02%甲酸为流动相,梯度洗脱,体积流量为0.4 m L·min-1,柱温为30℃,进样量为3μL。检测质谱采用电喷雾离子源(ESI)的飞行时间质谱,正、负离子模式下采集数据,全扫描的质量扫描范围m/z 100~800。结果:结合UPLC-QTOF/MS提供的化合物准确相对分子质量及其二级质谱数据、对照品信息、相关文献数据对活血通络粉针化学成分进行鉴定并对化合物的药材来源进行了归属,共鉴定出18个化学成分。结论:UPLC-QTOF/MS法快速、准确、全面地鉴定活血通络粉针中的多种成分,为其质控和药效物质基础研究提供一定的参考。展开更多
In the present study, an ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS) based chemical profiling approach to rapidly evaluate chemical diversity after co...In the present study, an ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS) based chemical profiling approach to rapidly evaluate chemical diversity after codecocting of the combination of Aconitum carmichaeli Debx.(wu-tou in Chinese, WT) and Bletilla striata(Thunb.) Reichb.f.(bai-ji in Chinese, BJ) incompatible pair. Two different kinds of decoctions, namely WT-BJ mixed decoction: mixed water extract of each individual herbs, and WT-BJ co-decoction: water extract of mixed two constituent herbs, were prepared. Batches of these two kinds of decoction samples were subjected to UPLC-QTOF/MS analysis, the datasets of tR-m/z pairs, ion intensities and sample codes were processed with supervised orthogonal partial least squared discriminant analysis(OPLS-DA) to holistically compare the difference between these two kinds of decoction samples. Once a clear classification trend was found in score plot, extended statistical analysis was performed to generate S-plot, in which the variables(tR-m/z pair) contributing most to the difference were clearly depicted as points at the two ends of "S", and the components that correlate to these ions were regarded as the most changed components during co-decocting of the incompatible pair. The identities of the changed components can be identified by comparing the retention times and mass spectra with those of reference compounds and/or tentatively assigned by matching empirical molecular formulae with those of the known compounds published in the literatures. Using the proposed approach, global chemical difference was found between mixed decoction and co-decoction, and hypaconitine, mesaconitine, deoxyaconitine, aconitine, 10-OH-mesaconitine, 10-OH-aconitine and deoxyhypaconitine were identified as the most changed toxic components of the combination of WT-BJ incompatible pair during co-decocting. It is suggested that this newly established approach could be used to practically reveal the possible toxic components changed/increased of the herbal combination taboos, e.g. the Eighteen Incompatible Medications(Shi Ba Fan), in traditional Chinese medicines.展开更多
基金the funding support from the Aid Program for Science and Technology Innovative Research Team in Higher Educational Institutions of Hunan Province([2010]212)Changsha City Science and Technology Project in 2015(k1501024-31)+3 种基金Key Discipline Program of State Administration of Traditional Chinese Medicine of the P.R.C([2009]30)Key Discipline in Hunan Province([2011]76)Provincial Natural Science Foundation of Hunan(2017JJ3234)Key Project of Science and Technology of Hunan Province(2016SK2033)
基金Financial supported by the National Natural Science Foundation of China (Grant No.81673872and 81460659)Department of Education Guangdong of Province (Grant No. YQ2013043)Department of Science and Technology of Tibet autonomous region (Grant No.2016ZR-ZY-01).
文摘目的:对小儿七星茶的主要化学成分进行解析和鉴定,并探讨其治疗小儿消化不良的作用机制。方法:采用UPLC-QTOF/MS技术对小儿七星茶进行测定分析。通过数据库搜索化学成分相关靶点和疾病相关靶点,并筛选出小儿七星茶对应的疾病治疗靶点。运用Cytoscape软件进行网络建立和分析,同时将成分和靶点根据药材来源进行归类,通过靶点数目分布验证组方的“君、臣、佐、使”配伍规律。运用ClueGo进行GO生物功能分析和KEGG通路富集,进一步预测小儿七星茶发挥药效的作用机制。结果:通过解析得到5 3 个化合物,筛选出疾病相关靶点6 3 个,其中AKT1、FOS、SLC6A4、COM T和5-H T受体是重要靶点,能调节碳水化合物消化吸收、5-H T代谢和cA M P等信号通路。结果表明,小儿七星茶能通过干预脑肠轴相关的靶点和通路发挥治疗作用。结论:本研究为小儿七星茶的深入研究提供了实验和理论基础,为中药复方的药效学机制研究提供了科学依据。
基金supported by the National Basic Research Program of China("973Program)(No2011CB505304)the Youth Scientific Research Project of Anhui Academy of Medical Science(YKY2018003)
文摘In the present study, an ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS) based chemical profiling approach to rapidly evaluate chemical diversity after codecocting of the combination of Aconitum carmichaeli Debx.(wu-tou in Chinese, WT) and Bletilla striata(Thunb.) Reichb.f.(bai-ji in Chinese, BJ) incompatible pair. Two different kinds of decoctions, namely WT-BJ mixed decoction: mixed water extract of each individual herbs, and WT-BJ co-decoction: water extract of mixed two constituent herbs, were prepared. Batches of these two kinds of decoction samples were subjected to UPLC-QTOF/MS analysis, the datasets of tR-m/z pairs, ion intensities and sample codes were processed with supervised orthogonal partial least squared discriminant analysis(OPLS-DA) to holistically compare the difference between these two kinds of decoction samples. Once a clear classification trend was found in score plot, extended statistical analysis was performed to generate S-plot, in which the variables(tR-m/z pair) contributing most to the difference were clearly depicted as points at the two ends of "S", and the components that correlate to these ions were regarded as the most changed components during co-decocting of the incompatible pair. The identities of the changed components can be identified by comparing the retention times and mass spectra with those of reference compounds and/or tentatively assigned by matching empirical molecular formulae with those of the known compounds published in the literatures. Using the proposed approach, global chemical difference was found between mixed decoction and co-decoction, and hypaconitine, mesaconitine, deoxyaconitine, aconitine, 10-OH-mesaconitine, 10-OH-aconitine and deoxyhypaconitine were identified as the most changed toxic components of the combination of WT-BJ incompatible pair during co-decocting. It is suggested that this newly established approach could be used to practically reveal the possible toxic components changed/increased of the herbal combination taboos, e.g. the Eighteen Incompatible Medications(Shi Ba Fan), in traditional Chinese medicines.
