基于UPLC-Q-TOF-MS/MS法的化痰合剂体外及入血成分分析  

Chemical constituents and absorbed components of Huatan mixture based on UPLC-Q-TOF-MS/MS

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作  者:孟慧頔 程雪梅[2] 党蕊 王长虹[2] 时扣荣[1] 刘娟[1] 范伟 罗兰 MENG Hui-di;CHENG Xue-mei;DANG Rui;WANG Chang-hong;SHI Kou-rong;LIU Juan;FAN Wei;LUO Lan(Department of Pharmacy,Seventh People’s Hospital of Shanghai University of Traditional Chinese Medicine,Shanghai 200137;Institute of Chinese Materia Medica,The MOE Key Laboratory for Standardization of Chinese Medicines,Shanghai Key Laboratory of Compound Chinese Medicine,Shanghai University of Traditional Chinese Medicine,Shanghai 201203)

机构地区:[1]上海中医药大学附属第七人民医院药学部,上海200137 [2]上海中医药大学中药研究所,中药标准化教育部重点实验室,上海市复方中药重点实验室,上海201203

出  处:《中南药学》2025年第1期84-93,共10页Central South Pharmacy

基  金:上海市浦东新区卫生健康委员会学科建设中药制剂转化医学项目(No.PWXx2020-04);上海市浦东新区卫生健康委员会学科建设中西医结合临床药学项目(No.PWZxk2022-07)。

摘  要:目的阐明化痰合剂的化学成分和口服吸收入血成分。方法在大鼠灌胃化痰合剂10 min、30 min、1 h、2 h、4 h、6 h、8 h后采集血清。采用UPLC-Q-TOF-MS/MS法测定,色谱柱为ACQUITY UPLC HSS T3柱(2.1 mm×100 mm,1.8μm);流动相:0.1%甲酸水(A)-乙腈(B),梯度洗脱;柱温45℃;流速0.3 mL·min^(-1);进样量5μL;电喷雾离子源(ESI);正、负离子模式检测。经Analyst TF 1.6采集数据,Peak View 1.2分析数据,根据保留时间、相对分子质量、一级和二级质谱数据,结合对照品和参考文献对化痰合剂及其口服入血的化学成分进行表征。结果从化痰合剂中共鉴定出133种成分,包括黄酮类67种、香豆素类22种、皂苷类15种、有机酸类14种、生物碱类3种、其他类12种;从含药血清中鉴定出15种成分。结论UPLC-Q-TOF-MS/MS法可较全面地鉴定化痰合剂中的化学成分和口服吸收入血成分,为化痰合剂的进一步研究提供依据。Objective To determine the chemical compositions and the absorbed components of Huatan mixture via oral administration.Methods Serum was collected from rats after gavage administration of Huatan mixture for 10 min,30 min,1 h,2 h,4 h,6 h and 8 h.The ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS/MS)method was performed on an ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8μm).The gradient elution was used with mobile phase of 0.1%formic acid in water(A)-acetonitrile(B).The column temperature was 45℃.The flow rate was 0.3 mL·min^(-1)and the injection volume was 5μL.The detection was performed with electrospray ionization(ESI)source in both positive and negative modes.The data were collected by Analyst TF 1.6 and then analyzed by Peak View 1.2.The chemical constituents and bioactive components were characterized according to the relative retention time,the relative molecular mass,and the first and second level mass spectrometry data in combination with the data of reference substance and literatures.Results Totally 133 components,including 67 flavonoids,22 coumarins,15 saponins,14 organic acids,3 alkaloids and 12 others were identified from Huatan mixture.Totally 15 components were identified from the serum after Huatan mixture administration.Conclusion The UPLC-Q-TOF-MS/MS can comprehensively identify the chemical constituents and bioactive components of Huatan mixture via oral administration,providing evidence for further research and development of Huatan mixture.

关 键 词:化痰合剂 化学成分 UPLC-Q-TOF-MS/MS 

分 类 号:R284.1[医药卫生—中药学]

 

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