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
Objective This study was conducted to develop an method for identification of Trachemys scripta elegans(Ba Xi Gui,巴西龟)shell glue from Chinemys reevesii(Zhong Hua Cao Gui,中华草龟)shell glue.Methods In this research...Objective This study was conducted to develop an method for identification of Trachemys scripta elegans(Ba Xi Gui,巴西龟)shell glue from Chinemys reevesii(Zhong Hua Cao Gui,中华草龟)shell glue.Methods In this research,an ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS)method coupled with Binary Compare tool of UNIFI software was validated to differentiate Trachemys scripta elegans(Ba Xi Gui,巴西龟)shell glue from Chinemys reevesii(Zhong Hua Cao Gui,中华草龟)shell glue.The gelatins were digested enzymatically into peptides using trypsin.The UPLC-QTOF/MS data of the trypsin digested samples was subjected to Binary Compare of UNIFI software in order to screen out the unique peptides.PEAKS■Studio software was utilized to identify the sequence of the marker peptides.Results It was found that m/z 641.3 was the marker peptide in samples of Trachemys scripta elegans(Ba Xi Gui,巴西龟)shell glue,and m/z 649.3 was the marker peptide in samples of Chinemys reevesii(Zhong Hua Cao Gui,中华草龟)shell glue,with possible amino acid sequence of GEAGPSGPAGPTGAR and GESGPSGPAGPTGAR respectively.Conclusions The results will be helpful for the differentiating between these 2 gelatins,and it can be also used for quality control of Tortoise shell glue(Gui Jia Jiao,龟甲胶).展开更多
Objective: To explore the main chemical compounds in Xiaoer Qixing Cha Formulae (XQCF), and investigate its mechanisms for the treatment of infantile functional dyspepsia (IFD). Methods: The chemical components were i...Objective: To explore the main chemical compounds in Xiaoer Qixing Cha Formulae (XQCF), and investigate its mechanisms for the treatment of infantile functional dyspepsia (IFD). Methods: The chemical components were identified by UPLC-QTOF/MS analytic technique. Targets of the compounds were screened from TCMSP and SWISS database, and disease targets were screened from OMIM and TTD online database. Candidate targets of compounds were mapped to the disease targets as predict therapeutic targets for XQCF. Several networks were constructed and analyzed by Cytoscape ver. 3.2.1. Meanwhile, prescription compatibility in XQCF was interpreted from the network perspective based on distribution of the number of targets. Furthermore, Gene Ontology (GO) enrichment analysis and KEGG pathway analysis were operated via Clue Go to illustrate complex relationships between the potential targets and pharmacological mechanisms. Results: A total of fifty-three compounds were recognized or tentatively characterized belonging to XQCF based on MS data and online chemical database. Sixty-three therapeutic targets were screened. AKT1, FOS, SLC6A4, COMT and 5-HT receptors were focused as therapeutic targets of XQCF. Pathways including carbohydrate digestion and absorption, serotonergic synapse, calcium signaling pathway and cAMP signaling pathway were predicted as significant regulatory pathways. The results indicated that the predicted targets and pathways related in brain-gut axis to a great extent, which could be potential pharmacological mechanism of XQCF for the treatment of IFD. Conclusions: The findings in this study provided the experimental and theoretical basis for further research for XQCF. Those also illustrated a reasonable method worth intensive study on pharmacodynamic mechanisms of TCM Formulae.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)
文摘Objective This study was conducted to develop an method for identification of Trachemys scripta elegans(Ba Xi Gui,巴西龟)shell glue from Chinemys reevesii(Zhong Hua Cao Gui,中华草龟)shell glue.Methods In this research,an ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS)method coupled with Binary Compare tool of UNIFI software was validated to differentiate Trachemys scripta elegans(Ba Xi Gui,巴西龟)shell glue from Chinemys reevesii(Zhong Hua Cao Gui,中华草龟)shell glue.The gelatins were digested enzymatically into peptides using trypsin.The UPLC-QTOF/MS data of the trypsin digested samples was subjected to Binary Compare of UNIFI software in order to screen out the unique peptides.PEAKS■Studio software was utilized to identify the sequence of the marker peptides.Results It was found that m/z 641.3 was the marker peptide in samples of Trachemys scripta elegans(Ba Xi Gui,巴西龟)shell glue,and m/z 649.3 was the marker peptide in samples of Chinemys reevesii(Zhong Hua Cao Gui,中华草龟)shell glue,with possible amino acid sequence of GEAGPSGPAGPTGAR and GESGPSGPAGPTGAR respectively.Conclusions The results will be helpful for the differentiating between these 2 gelatins,and it can be also used for quality control of Tortoise shell glue(Gui Jia Jiao,龟甲胶).
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Objective: To explore the main chemical compounds in Xiaoer Qixing Cha Formulae (XQCF), and investigate its mechanisms for the treatment of infantile functional dyspepsia (IFD). Methods: The chemical components were identified by UPLC-QTOF/MS analytic technique. Targets of the compounds were screened from TCMSP and SWISS database, and disease targets were screened from OMIM and TTD online database. Candidate targets of compounds were mapped to the disease targets as predict therapeutic targets for XQCF. Several networks were constructed and analyzed by Cytoscape ver. 3.2.1. Meanwhile, prescription compatibility in XQCF was interpreted from the network perspective based on distribution of the number of targets. Furthermore, Gene Ontology (GO) enrichment analysis and KEGG pathway analysis were operated via Clue Go to illustrate complex relationships between the potential targets and pharmacological mechanisms. Results: A total of fifty-three compounds were recognized or tentatively characterized belonging to XQCF based on MS data and online chemical database. Sixty-three therapeutic targets were screened. AKT1, FOS, SLC6A4, COMT and 5-HT receptors were focused as therapeutic targets of XQCF. Pathways including carbohydrate digestion and absorption, serotonergic synapse, calcium signaling pathway and cAMP signaling pathway were predicted as significant regulatory pathways. The results indicated that the predicted targets and pathways related in brain-gut axis to a great extent, which could be potential pharmacological mechanism of XQCF for the treatment of IFD. Conclusions: The findings in this study provided the experimental and theoretical basis for further research for XQCF. Those also illustrated a reasonable method worth intensive study on pharmacodynamic mechanisms of TCM Formulae.
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.
