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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
【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,1.8 μm);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5 μL;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。
【Abstract】 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,1.8 μm).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 5 μL.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.
【Key words】 Huatan mixture; chemical composition; UPLC-Q-TOF-MS/MS;
- 【文献出处】 中南药学 ,Central South Pharmacy , 编辑部邮箱 ,2025年01期
- 【分类号】O657.63;R284.1
- 【下载频次】145