院内制剂消炎抗菌片的UPLC-LTQ-Orbitrap HRMS分析

目的：采用UPLC-LTQ-Orbitrap HRMS方法鉴定消炎抗菌片中的主要成分。方法：选用Kromasil C₁₈色谱柱（250 mm×4.6 mm，5 μm），流动相为甲醇和水，梯度洗脱，流速为1 mL·min^-1，进样量1 μL，柱温为35℃，采用正、负离子检测模式。结果：通过相关文献及质谱数据，共鉴定出30个成分，分别为16个黄酮类化合物、10个鞣质类化合物、1个三萜类化合物，2个有机酸类化合物和1个酚类化合物。结论：本研究首次建立UPLC-LTQ-Orbitrap HRMS技术对消炎抗菌片的主要成分进行鉴定，为消炎抗菌片的药效成分研究提供科学依据。     

基于UPLC-Q-TOF/MS技术的三黄片化学成分解析

目的：采用超高效液相色谱-四级杆飞行时间质谱（UPLC-Q-TOF/MS）串联技术对三黄片化学成分进行解析鉴定。方法：采用Acquity UPLC^TM BEH C₁₈色谱柱（100 mm×2.1 mm，1.7 μm），以甲醇-0.1%甲酸水溶液为流动相对三黄片95%乙醇提取物中各成分进行快速分离；采用配备电喷雾离子源的Waters Q-TOF Xevo G2质谱仪，运用正负离子扫描模式对样品中各成分进行高分辨检测。对于已知成分，根据对照品色谱保留时间和质谱裂解规律进行确证；对于未知化合物，则根据其准确的相对分子量、二级特征碎片离子，并进一步结合相关文献进行推测。对三黄片各化合物来源也进行了归属。结果：共解析鉴定出28个化学成分，包括8个蒽醌类化合物，18个黄酮类化合物，1个多酚类成分和1个生物碱类成分。结论：UPLC-Q-TOF/MS能快捷、准确地鉴定三黄片化学成分，研究结果可为三黄片药动学、代谢产物推测、药效物质基础及作用机制等研究提供科学的参考依据。     

基于UPLC-Q-TOF-MS技术的五酯胶囊及其入血原型木脂素类成分快速鉴定分析

目的：利用超高效液相色谱-飞行时间质谱联用（UPLC-Q-TOF-MS）技术通过特征碎片和中性丢失快速鉴别五酯胶囊及其入血的原型木脂素类成分。方法：ACQUITY UPLC BEH C₁₈色谱柱（100 mm×2.1 mm,1.7 μm）,以0.1%甲酸水-甲醇梯度洗脱,流速0.2 mL·min^-1;进样量2 μL。电喷雾离子源（ESI）,正离子模式下采集。结果：结合文献及对照品的色谱、质谱裂解行为,共推测鉴定五酯胶囊中木脂素类化合物14个,其中入血成分8个。结论：本研究建立了UPLC-Q-TOF-MS法对五酯胶囊及其入血原型木脂素类成分进行分析,为阐明其药效物质基础和作用机制提供参考。     

运用UPLC-BCD方法快速筛选中草药中凝血酶抑制剂

目的：建立超高相液相色谱-生物化学检测（UPLC-BCD）分析方法快速筛选丹参、远志、蕲艾药材中凝血酶抑制剂,为中草药中生物活性成分的辨识提供一种便捷的技术手段。方法：运用UPLC分析技术,采用Xtimate UHPLC C₁₈色谱柱（2.1 mm×100 mm,1.8 μm）,柱温30 ℃,流动相为甲醇（B）-0.1%甲酸水溶液（A）,梯度洗脱,检测波长256 nm,体积流量0.2 mL·min^-1。以比伐卢定作为阳性对照,考察酶反应条件,建立UPLC-BCD分析方法检测3种药材提取物与凝血酶反应前后色谱特征图谱及酶反应产物的差异,评价3种药材凝血酶抑制作用、快速筛选所含酶抑制剂,采用超高效液相色谱-离子阱-静电场轨道阱质谱（UHPLC-LTQ/Orbitrap MS）方法鉴定酶抑成分。结果：丹参、远志和蕲艾均具有较好的凝血酶抑制作用,检出丹参和远志中7种酶抑制剂,初步鉴定为丹酚酸A、迷迭香酸、丹酚酸B、西伯利亚远志呫吨酮B、远志山酮Ⅲ、3,6’-二芥子酰基蔗糖、细叶远志苷A。蕲艾色谱峰在反应前后无明显变化,其酶抑制活性可能来源于色谱图未显示的其他成分。结论：建立的UPLC-BCD方法能够快速辨别复杂基质的酶抑制作用及酶抑制剂,为中草药中生物活性成分的快速筛选提供了快速、便捷的分析手段。     

基于HPLC指纹图谱结合多种化学模式识别评价生脉饮(党参方)质量

目的：建立多批次生脉饮（党参方） HPLC指纹图谱并采用多种化学计量学分析评价多厂家多批次生脉饮（党参方）的整体质量。方法：采用Ultimate XB-C₁₈色谱柱（4.6 mm×250 mm,5 μm）,流动相为乙腈-0.15%甲酸水溶液,检测波长为260 nm,流速0.8 mL·min^-1,柱温20℃,对多批不同厂家和来源的生脉饮（党参方）制剂进行分析,建立中药色谱指纹图谱,并结合聚类分析、主成分分析与偏最小二乘法判别分析对生脉饮（党参方）质量进行评价。结果：建立了生脉饮（党参方） HPLC指纹图谱,确定了23个共有峰,并指认了其中7个色谱峰;多批次生脉饮（党参方） HPLC指纹图谱的相似度为0.061~0.798;聚类分析与主成分分析结果一致,结合正交偏最小二乘法判别分析发现3类主成分中包含的7个成分峰是造成不同批次生脉饮（党参方）质量差异的主要标志物。在多指标成分定量分析方法学考察结果中,7种指标性成分的加样回收率在97.32%~101.26%,RSD为1.89%~3.56%。结论：不同批次的生脉饮（党参方）之间虽有一定的相关性,但存在质量差异。生脉饮（党参方）检测方法的建立可以为其质量控制及评价提供参考依据,且具有一定的药用开发价值,为其进一步药效及制剂研究奠定基础。     

清肝利胆口服液化学成分的鉴定及网络药理学法探讨其作用机制

目的：对清肝利胆口服液中的化学成分进行鉴定,探索其保肝利胆的作用机制。方法：采用超高效液相色谱-四级杆-飞行时间质谱（UPLC-Q-TOF-MS/MS）法鉴定清肝利胆口服液中所含的化学成分;利用TCMSP、TTD等数据库获得所得成分和疾病分别相对应的靶点信息;通过生物信息学技术富集涉及的相关通路及生物过程,并运用Cytoscape软件进行构图。结果：鉴定出清肝利胆口服液成分22种,成分作用靶点548个,疾病靶点454个,主要作用通路5条。结论：清肝利胆口服液中化学成分可以通过UPLC-Q-TOF-MS/MS法进行简便、快速定性分析,而其发挥保肝利胆的作用可能与抗炎、免疫调节、细胞色素P450代谢和血糖调节相关。     

基于液质联用法对白及中2-异丁基苹果酸葡萄糖氧基苄酯类成分的定性定量分析

目的： 建立白及中2-异丁基苹果酸葡萄糖氧基苄酯类成分的UPLC-ESI-Q/TOF-MS快速识别鉴定方法,以及主成分militarine的UPLC测定方法。方法： 液质联用方法采用Waters Acquity UPLC BEH C₁₈（1.7 μm,2.1 mm×100 mm）色谱柱,乙腈-0.1%甲酸溶液梯度洗脱,检测器为高分辨四极杆飞行时间质谱,ESI离子源,MS^E（^E代表碰撞能量）采集方式,采集质量数范围m/z 100~1 000。含量测定采用UPLC法,以乙腈-0.1%磷酸溶液（22：78）为流动相;检测波长为223 nm;柱温：35℃;流速：0.2 mL·min^-1。结果： 利用建立的白及化学成分数据库,结合2-异丁基苹果酸葡萄糖氧基苄酯类成分的诊断离子、准确分子量、质谱碎片及对照品信息,快速分析鉴定21个目标化合物。主成分militarine在19.059 0~381.180 8 μg·mL^-1范围内线性关系良好（r=0.998 6）。加样回收率为100.9%,RSD为1.5%。36批白及中militarine的含量范围是1.5%~4.6%。结论： UPLC-Q/TOF-MS法能快速、准确地鉴定白及中的化学成分,为其药效物质基础研究提供科学依据。建立的UPLC含量测定方法操作简便、准确可靠,可用于白及的质量控制。     

基于高效液相色谱指纹图谱的多叶棘豆指标成分的含量测定

目的： 建立多叶棘豆HPLC指纹图谱及2个指标成分的含量测定方法。方法： 采用HPLC法,Symmetry^®C₁₈色谱柱（250 mm×4.6 mm,5.0 μm）;以乙腈（A）-0.1%乙酸水溶液（B）梯度洗脱;柱温30℃;流速为1.0 mL·min^-1;检测波长为254 nm。结果： 建立了10批多叶棘豆药材的HPLC指纹图谱,相似度在0.937~0.973,共标定了18个共有峰;同时测定了24批药材中槲皮素-7-O-α-鼠李糖-3-O-（6″-反式咖啡酰）-β-D-葡萄糖基-（1→2）-β-D-葡萄糖苷和芦丁的含量,分别为0.02~11.75 mg·g^-1和0.01~1.26 mg·g^-1。结论： 建立的指纹图谱结合含量测定的方法可有效、全面地用于多叶棘豆药材的质量评价。     

UPLC-QE-Orbitrap-MS法同时测定忍冬叶中10个活性成分

目的：建立UPLC-QE-Orbitrap-MS法,同时测定忍冬叶中10个活性成分（新绿原酸,断马钱子酸,绿原酸,断氧化马钱苷,芦丁,忍冬苷,木犀草苷,异绿原酸A,异绿原酸C,木犀草素）的含量。方法：采用Phenomenex Luna Omega C₁₈（2.1 mm×100 mm,1.6 μm）色谱柱,流动相为乙腈-0.1%甲酸水,梯度洗脱,流速0.2 mL·min^-1,柱温30℃;质谱条件：电喷雾离子源（ESI源）,扫描方式采用正、负离子全扫模式（Full MS/dd-MS²）。结果：10个成分在考察的浓度范围内呈现良好的线性关系（R²>0.993）,平均加样回收率94.3%~101.5%,RSD<3.4%。10批忍冬叶样品中上述10个成分的含量范围分别在1.50~3.92,4.01~16.66,10.91~26.93,3.52~22.73,0.02~1.08,2.48~10.57,2.23~13.06,2.80~29.89,1.79~7.00,0.18~0.61 mg·g^-1之间。10个成分在10批忍冬叶样品中的含量相差数倍至50倍,不同产地忍冬叶样品质量差异非常显著。结论：该方法准确可行,结果稳定可靠,可用于忍冬叶样品中多种主要活性成分的含量测定。     

基于UHPLC-Q-Orbitrap HRMS的参松养心胶囊化学成分识别及作用机制研究

目的：为系统研究复方中药制剂参松养心胶囊的化学成分组成,同时探讨其发挥疗效的主要作用机制与疾病类型。方法：采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱（UHPLC-Q-Orbitrap HRMS）对参松养心胶囊中的主要化学成分进行快速定性分析,色谱柱采用Waters ACQUITY UPLC BEH C₁₈色谱柱（2.1 mm×50 mm,1.7 μm）,流动相为乙腈（A）-0.1%甲酸水（B）溶液,梯度洗脱,流速为0.2 mL·min^-1。通过捕捉未知化合物的精确分子质量及多级碎片离子信息,同时与标准品进行比对,并结合相关参考文献以及Mass Bank等网络数据库信息从而实现对未知物的准确快速定性。在此基础上,采用网络药理学方法,对药物成分进行靶标预测、功能研究及疾病富集,从而阐明其主要作用机制。结果：从参松养心胶囊中共鉴定出化合物39种,基于鉴定的化学成分共得到潜在靶标190个。靶标功能富集分析结果表明,参松养心胶囊主要从对血管内皮、血管平滑肌、心肌、炎症以及血小板等方面,综合发挥其活血通络、益气养阴、清心安神的功效。结论：本研究结合UHPLC-Q-Orbitrap HRMS质谱分析与网络药理学研究方法,为参松养心胶囊的有效成分识别、质量标志物的筛选及明确其作用机制提供了重要参考依据。     

基于UPLC-Q-Exactive Orbitrap-MS联合网络药理学探究双黄连解热抗炎的作用机制

目的:基于UPLC-Q-Exactive Orbitrap-MS方法,利用网络药理学和分子对接技术初步探究双黄连解热抗炎的物质基础及作用机制.方法:利用UPLC-Q-Exactive Orbitrap-MS技术鉴定双黄连口服液中的主要化学成分.基于网络药理学,将已定性化合物录入Swiss Target数据库筛选成分靶点...     

Two new constituents from mangrove Bruguiera gymnorrhiza

A lignan and two aromatic compounds were isolated from the branches of the mangrove plant, Bruguiera gymnorrhiza. They were brugunin A (1), bruguierol D (2) and 2,3-dimethoxy-5-propylphenol (3). Among them, 1 and 2 were new compounds; 3 was isolated from a natural source for the first time. The structures of these compounds were determined by NMR spectroscopic studies as well as chemical evidence.     

A new triterpenoid from Entodon okamurae Broth

One new triterpenoid, entokamurol (1), was isolated from Entodon okamurae Broth, together with other nine compounds, namely dryocrassol (2), chrysophamol (3), physcion (4), 10-nonacosamnol (5), n-hexadecanol (6), phthalic acid isodibutyl ester (7), curcumol (8), β-sitosterol (9) and daucosterol (10). Their structures were elucidated on the basis of extensive NMR (DEPT, DQF-COSY, HMQC, HMBC and NOESY), IR and MS studies. All the compounds were isolated and identified from the genus of Entodon for the first time, and it is also the first report of a guaiane-type sesquiterpenoid and compounds with anthraquinone skeleton in mosses.     

Rearranged abietane diterpenoids from Clerodendrum mandarinorum

Five new abietane derivatives which have a commonly rearranged abietane skeleton contained a 17(15 → 16),18(4 → 3)-diabeo-abietane framework, mandarones D-H, were isolated from the stem of Clerodendrum mandarinorum Diels (Verbenaceae). The structures were characterized as (16S)-12,16-epoxy-11-hydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13-pentaene-7-one (mandarone D, 1), 12,16-epoxy-11,14-dihydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-7-one (mandarone E, 2), 12,16-epoxy-6,11,14-trihydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-7-one (mandarone F, 3), 12,16-epoxy-11,14-dihydroxy-6-methoxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-2,7-dione (mandarone G, 4) and 12,16-epoxy-11,14-dihydroxy-17(15 → 16),18(4 → 3)-diabeo-abieta-3,5,8,11,13,15-hexaene-1,7-dione (mandarone H, 5) respectively, mainly based on the spectral analysis and by comparison with those of closely related compounds.     

Chemical Constituents from the Leaves of Magnolia Denudata

20 compounds were isolated from the leaves of Magnolia denudata including 16 lignans, which belong to 6 structural types. Except for (7R, 8S, 1'S) -δ^8' - 1', 4' - dihydro - 5'- methoxy - 3, 4 -methylenedioxy - 4' - oxo -7.O.2', 8.1' - neolignan (6), magliflonenone (9), 2,5' - diene-2', 8'- epoxy - 5' - methoxy - 8 - methyl - 4' - oxo - 3,4-methylenedioxy - spiro (5,5) - undecane (10), veraguensin (16) and β-sitosterol (20), the other 15 compounds were obtained from this species for the first time. The absolute configurations of 3 compounds (1,4,10) were determined by CD spectroscopy for the first time. The anti-inflammatory activities of compounds 1, 2 and 16 were assessed and 2 was shown to have significant inhibition effect on mice hind-paw edema induced by carrageenan.     

A new meroditerpenoid from Mayodendron igeum

A new meroditerpenoid, igeumone (1), together with 18 known compounds (2-19), were isolated from ethanolic extract of the bark of Mayodendron igeum. Their structures were determined by analysis of spectral data or comparison with authentic samples. X-ray crystallographic analysis was employed to unambiguously determine the structure of 1.     

Studies on chemical constituents from Ilex pubescens

Two new phenolic glycosides, ilexpubsides A and B, along with four known lignan glycosides were isolated from the roots of Ilex pubescens. By spectral evidence, the structures of the new compounds were elucidated as 4-O-β-D-[6'-O-(4'-O-β-D-glucopyranosylvanilloyl)glucopyranosyl] vanillic acid (1) and syringinic 6'-O-β-D-xylopyranoside (2). The known compounds were identified to be liriodendrin (3), (-)-olivil (4), tortoside A (5) and (+)-cyclo-olivil (6). All compounds were first isolated from Ilex pubescens.     

Chemical constituents from Cimicifuga foetida

From the rhizoma of Cimicifuga foetida L. (Ranunculaceae) a new chromone, 6'-hydroxylangelicain (18), has been isolated together with 20 known compounds. The structure of 18 has been elucidated on the basis of spectroscopic and chemical evidence.     

A New Bicoumarin from Stellera Chamaejasme L

Thirteen compounds were isolated from roots of Stellera chamaejasme L. (Thymelaeaceae). They are β-sitosterol (2), simplexin (3), pimelea factor P2 (4), daucosterol (5), (+)-3-hydroxy-1,5-diphenyl-1-pentanone (6), 4-ethoxy-benzoic acid (7), 2,4,6-Trimethoxy-benzoic acid (8), (+)-afzelechin (9), fumaric acid (10), N,N-dimethyl-L-aspartic acid (11), umbelliferone (12), daphniretin (13) and a novel bicoumarin named bicoumastechamin (1). Among the known compounds, 7, 8, 9, 10 and 11 were first isolated from this plant, and 6 was first isolated from the natural resources. Their structures have been elucidated on the basis of spectral data. In vitro bioassays showed that 4 inhibited cancer cell growth, 13 exhibited immunomodulatory activity, and 6 exhibited both immunomodulatory and anti-tumor activity.     

Antibacterial constituents from Stemona sessilifolia

Bioassay-guided fractionation led to the isolation of eight compounds from Stemona sessilifolia. Of the eight isolates, three new bibenzyls, stilbostemins M-O (1-3), and a new tocopherol, 6-methoxy-3,4-dehydro-δ-tocopherol (4) were revealed together with four known compounds 3,5-dihydroxy-2'-methoxy bibenzyl (5), 3,5-dihydroxy bibenzyl (6), β-tocopherol (7), and γ-tocopherol (8). Compounds 5, 6, and 8 exhibited strong antibacterial activities against Staphylococcus aureus and S. epidermidis.