基于UPLC-Q-TOF-MS技术的脉络宁注射液酯提废渣大孔树脂富集液的化学成分鉴定和含量测定

Chemical composition and content determination in macroporous resin enrichment solution from ester extraction residue of Mailuoning injection based on UPLC-Q-TOF-MS

目的利用超高效液相-四极杆串联飞行时间质谱(UPLC-Q-TOF-MS)技术分析脉络宁注射液酯提废渣的化学成分,为酯提废渣资源的再利用提供科学依据。方法利用ASD-7大孔树脂柱富集脉络宁注射液酯提废渣化学成分,采用UPLC-Q-TOF-MS技术对脉络宁注射液酯提废渣大孔树脂富集液进行数据采集和化学成分鉴定,采用定量软件对绿原酸、异绿原酸、异绿原酸C、灰毡毛忍冬皂苷甲和灰毡毛忍冬皂苷乙进行含量测定。结果共鉴定出脉络宁注射液酯提废渣中42个化学成分,包括9个酚酸类化合物、9个黄酮类化合物、10个环烯醚萜类化合物、8个三萜皂苷类化合物、5个苯丙素类化合物和1个联苄类化合物,定量分析结果显示绿原酸、异绿原酸、异绿原酸C、灰毡毛忍冬皂苷甲和灰毡毛忍冬皂苷乙在考察的浓度范围内与峰面积线性关系良好(r>0.9990),精密度、重复性和稳定性良好,加样回收率为95.38%~103.06%,RSD为0.76%~1.8%。结论本研究可用于脉络宁注射液酯提废渣大孔树脂富集液中化学成分的鉴定以及5种有效成分的准确定量分析,为脉络宁注射液酯提废渣的再利用和制备工艺奠定基础。

Objective To identify chemical components and determine the content in macroporous resin enrichment solution from ester extraction residue of Mailuoning injection by ultraperformance liquid chromatography quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS)technology,and to provide a scientific basis for the reuse of ester extraction residue of Mailuoning injection.Methods Mailuoning injection ester extraction residues were enriched by ASD-7 macroporous resin columns.UPLC-Q-TOF-MS technology was used to collect the data and identify chemical components in it,and the content were determined by quantitative software.Results Totally 42 chemical components were identified,including 9 phenolic acids,9 flavonoids,10 iridoids,8 triterpenoid saponins,5 phenylpropanoids,and 1 dibenzyl.UPLC-Q-TOF-MS was used to quantitatively analyze the contents of chlorogenic acid,isochlorogenic acid A,isochlorogenic acid C,macranthoidin A and macranthoidin B.The linearity was good(r>0.9990),the precision,repeatability and stability were good,the recovery ranged 95.38%~103.06%,and the RSD was 0.76%~1.8%.Conclusion The method for the chemical components can identify the chemical components and accurately quantify the 5 effective components in macroporous resin enrichment solution from Mailuoning injection ester extraction residues,laying a foundation for the reuse and preparation of Mailuoning injection ester extraction residues.