基于UPLC-QE-Orbitrap-MS/MS技术分析新疆鼠尾草乙酸乙酯提取物化学成分及入血成分  

Analysis of chemical and hematogenous components of ethyl acetate extract from Salvia deserta in Xinjiang Using UPLC-QE Orbitrap MS/MS Technology

作　　者：王启文 王蕾 李雨欣 刘忠毅 王晓梅[1] 胡君萍[1] 丛媛媛[1] 王新玲[1] WANG Qiwen;WANG Lei;LI Yuxin;LIU Zhongyi;WANG Xiaomei;HU Junping;CONG Yuanyuan;WANG Xinling(College of Pharmacy,Xinjiang Medical University,Urumqi 830017,China)

机构地区：[1]新疆医科大学药学院,乌鲁木齐830017

出　　处：《新疆医科大学学报》2024年第10期1406-1417,1430,共13页Journal of Xinjiang Medical University

基　　金：国家自然科学基金地区项目(82060771);新疆天然药物有效成分与药物释放技术重点实验室项目(XJDX1713)。

摘　　要：目的采用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UPLC-QE-Orbitrap-MS/MS)技术分析新疆鼠尾草乙酸乙酯提取物(Ethyl acetate extraction of Salvia deserta Schang,SDS-EE)的化学成分及入血成分。方法新疆鼠尾草根加20倍量95%乙醇,85℃回流提取3次,每次2.5 h,浓缩得醇提浸膏,加水混悬后,再加等比例的乙酸乙酯萃取5次即得SDS-EE。取SD大鼠12只,随机分成空白组和给药组,每组6只。给药组灌胃给予SDS-EE溶液160 mg·kg^(-1)·d^(-1),空白组灌胃给予相同体积0.5%CMC-Na溶液,连续给药20 d。采用三氯化铁诱导建立SD大鼠血栓模型,腹主动脉取血并收集血清样品。采用ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm),以0.1%甲酸乙腈溶液(A)-0.1%甲酸水溶液(B)为流动相进行梯度洗脱,流速0.5 mL/min,进样量5μL,采用UPLC-QE-Orbitrap-MS/MS技术,利用Orbitrap Exploris 120质谱,在正、负离子两种模式下获取SDS-EE和血清样品中化合物的相对分子质量、二级质谱裂解碎片离子信息和保留时间,结合相关文献、对照品比对和数据库信息,分析鉴定SDS-EE和吸收入血的化学成分。结果从SDS-EE中共鉴定出52个化合物,包括7个苯丙素类、3个香豆素类、12个萜类、7个酚酸类、3个醌类、5个醛类、5个黄酮类、9个有机酸类和1个其它类。鉴定出入血成分11个,其中9个为原型成分,2个是代谢产物,其主要代谢途径为氧化反应。结论通过UPLC-QE-Orbitrap-MS/MS技术快速分析了新疆鼠尾草SES-EE的化学成分及入血成分。Objective To analyze the chemical components and blood constituents of the ethyl acetate extractionof Salvia deserta Schang(SDS-EE)using ultra-high-performance liquid chromatography combined with quadrupole-electrostatic field orbitrap high-resolution tandem mass spectrometry(UPLC-QE-Orbitrap-MS/MS)technology.Methods The Salvia deserta Schang root was extracted with 20 volumes of 95%ethanol,refluxed at 85℃for 3 periods of 2.5 hours each,concentrated to obtain the alcohol-extracted extract,mixed with water and then extracted with an equal proportion of ethyl acetate for 5 periods to obtain the SDS-EE.A total of 12 SD rats were randomly assigned to 2 groups:the blank group and the drug-administered group,with 6 rats in each.The drug group was administered 160 mg·kg^(-1)·d^(-1) of SDS-EE solution via gavage,while the blank group received an equivalent volume of 0.5%CMC-Na solution via gavage for a 20-day period.A thrombus model was constructed in SD rats using ferric trichloride,and blood samples were collected from the abdominal aorta,along with serum samples.An ACQUITY UPLC BEH C_(18) column(2.1 mm×100 mm,1.7μm)was used for gradient elution with 0.1%formic acid acetonitrile solution(A)-0.1%formic acid aqueous solution(B)as the mobile phase,at a flow rate of 0.5 mL/min with an injection volume of 5μL.Utilizing UPLC-QE-Orbitrap-MS/MS technology with the Orbitrap Exploris 120 mass spectrometer,the relative molecular masses,secondary mass spectrometry fragmentation ion information,and retention times of the compounds in SDS-EE and serum samples were obtained in both positive and negative ion modes.By combining relevant literature,reference substance comparison,and database information,the chemical constituents of SDS-EE and those absorbed into the blood were analyzed and identified.Results A total of 52 compounds were identified from SDS-EE,including 7 phenylpropanoids,3 coumarins,12 terpenoids,7 phenolic acids,3 quinones,5 aldehydes,5 flavonoids,9 organic acids and 1 other class.11 blood-borne components were

关 键 词：新疆鼠尾草 乙酸乙酯提取物 超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法 药效物质基础 入血成分 

分 类 号：R965[医药卫生—药理学]