摘要
目的建立全面、快速分析当归中苯酞类和有机酸类等化学成分的方法,为当归的质量评价和药效物质研究提供科学依据。方法以当归70%乙醇提取液为分析样品,采用超高效液相色谱-四极杆-飞行时间串联质谱联用技术进行分析。色谱柱为ACQUITY UPLCBEH-C18,流动相为0.1%甲酸溶液-乙腈溶液(梯度洗脱),流速为0.3 mL/min,柱温为30℃,进样量为2μL。离子源为电喷雾离子源,采用正离子扫描模式,质量扫描范围为m/z 50~1000;毛细管电压为4000 V;雾化器压力为35 psi;裂解电压为135 V,锥孔电压为65 V;干燥气温度为320℃;干燥气流量为10 L/min,鞘流气流量为11 L/min;碰撞能量为20、40 V。使用Qualitative Analysis 10.0软件获取化合物的保留时间、准分子离子峰的精确质量数及二级碎片等信息,通过与对照品质谱图比对,并结合相关文献报道、质谱裂解规律及Chemspider、MassBank、PubChem等数据库信息对化合物进行分析。结果从当归提取物中共鉴定或推断出72个化合物,包括苯酞类化合物55个、有机酸类化合物13个、其他类化合物4个。结论成功建立了能快速、准确识别与鉴定当归中有机酸类和苯酞类等化学成分的方法,为其化学成分的全面表征提供了一种高效、快速的分析手段。
OBJECTIVE To establish a comprehensive and rapid method for the analysis of chemical constituents as phthalides and organic acids in Angelica sinensis,and to provide scientific reference for the quality evaluation and pharmacodynamic substance research of A.sinensis.METHODS The 70%ethanol extract of A.sinensis was analyzed by ultra high performance liquid chromatography-quadrupole-time of flight tandem mass spectrometry(UPLC-Q-TOF/MS).The determination was performed on ACQUITY UPLC BEH-C18 column with mobile phase consisted of 0.1%formic acid solution-acetonitrile(gradient elution)at the flow rate of 0.3 mL/min.The column temperature was set at 30℃,and sample size was 2μL.The ion source was an electrospray ion source,using positive ion scanning mode,and the mass scanning range was m/z 50-1000.Capillary voltage was 4000 V;atomizer pressure was 35 psi;cracking voltage was 135 V and the taper hole voltage was 65 V;the temperature of dry gas was 320℃;the flow of dry gas was 10 L/min and the flow of sheath gas was 11 L/min;collision energy were 20 and 40 V.Qualitative Analysis 10.0 software was used to obtain the retention time of compounds,the accurate mass number of excimer ion peaks and secondary fragments.The compounds were analyzed by comparing with the mass spectra of the reference substance,combined with relevant literature,mass spectrometry cleavage law and database such as Chemspider,MassBank,PubChem.RESULTS A total of 72 compounds were identified or deduced from A.sinensis,including 55 phthalides,13 organic acids and 4 other constituents.CONCLUSIONS The established method is rapid and accurate for the identification of chemical constituents from A.sinensis,such as organic acids and phthalides,which provides an efficient and rapid analytical method for the comprehensive characterization of its chemical constituents.
作者
张清清
冯媛
李春花
李国川
刘兴超
李颢玥
王红芳
周莉
张一昕
ZHANG Qingqing;FENG Yuan;LI Chunhua;LI Guochuan;LIU Xingchao;LI Haoyue;WANG Hongfang;ZHOU Li;ZHANG Yixin(College of Pharmacy,Hebei University of Chinese Medicine,Shijiazhuang 050200,China;Hebei TCM Formula Preparation Technology Innovation Center,Shijiazhuang 050091,China;Hebei Traditional Chinese Medicine Processing Technology Innovation Center,Shijiazhuang 050091,China)
出处
《中国药房》
CAS
北大核心
2022年第5期579-585,591,共8页
China Pharmacy
基金
河北省自然科学基金资助项目(No.H2019423103)
河北中医学院优秀青年教师基础研究计划项目(No.YQ2018008)。
