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Identification and characterization of phenolics and terpenoids from ethanolic extracts of Phyllanthus species by HPLC-ESI-QTOF-MS/MS 被引量:10
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作者 Sunil Kumar Awantika Singh Brijesh Kumar 《Journal of Pharmaceutical Analysis》 SCIE CAS CSCD 2017年第4期214-222,共9页
Phyllanthus species plants are a rich source of phenolics and widely used due to their medicinal properties. A liquid chromatography–tandem mass spectrometry(LC–MS/MS) method was developed using high-pressure liquid... Phyllanthus species plants are a rich source of phenolics and widely used due to their medicinal properties. A liquid chromatography–tandem mass spectrometry(LC–MS/MS) method was developed using high-pressure liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry(HPLC-ESI-QTOFMS/MS) for the identification and characterization of quercetin, kaempferol, ellagic acid and their derivatives in ethanolic extracts of Phyllanthus species. The chromatographic separation was carried out on Thermo Betasil C_8 column(250 mm×4.5 mm, 5 μm) using 0.1% formic acid in water and 0.1% formic acid in methanol as the mobile phase. The identification of diagnostic fragment ions and optimization of collision energies were carried out using 21 reference standards. Totally 51 compounds were identified which include 21 compounds identified and characterized unambiguously by comparison with their authentic standards and the remaining 30 were tentatively identified and characterized in ethanolic extracts of P. emblica, P. fraternus, P. amarus and P.niruri. 展开更多
关键词 PHYLLANTHUS SPECIES hplc-esi-qtof-ms/MS Phenolics
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α-Glucosidase Inhibitory Activity-guided Identification of Compounds from Clerodendrum bungei Steud by HPLC-ESI-QTOF-MS/MS 被引量:1
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作者 HUANG Xiao-Long WAN Dan +3 位作者 SHU Jun FANG Liang-Zi ZOU Du-Zhun ZHANG Shui-Han 《Digital Chinese Medicine》 2019年第1期41-49,共9页
Objective To identify the compounds withα-glucosidase inhibitory activity from Clerodendrum bungei Steud(Chou Mu Dan,臭牡丹)using HPLC-ESI-QTOF-MS/MS.Methods The ethanol extracts of Clerodendrum bungei Steud(Chou Mu ... Objective To identify the compounds withα-glucosidase inhibitory activity from Clerodendrum bungei Steud(Chou Mu Dan,臭牡丹)using HPLC-ESI-QTOF-MS/MS.Methods The ethanol extracts of Clerodendrum bungei Steud(Chou Mu Dan,臭牡丹)were partitioned with petroleum ether,ethyl acetate,n-butanol,and water.The assay forα-glucosidase inhibitory activity revealed strongα-glucosidase inhibitory activity in the ethyl acetate fraction,and the bioactive compounds present in this fraction were identified by the HPLCESI-QTOF-MS/MS method.Results A total of 29 compounds were determined,among the identified bioactive components;these included 12 phenylethanoid glycosides(compounds 5,6,17,20-22,24),7 flavonoids(compounds 10,19,23,25-28),5 phenolic acids(compounds 2-4,7,9),and 5 other compounds.Compounds 2-4,7,9-10,12-13,15,19,and 26,with a potentialα-glucosidase inhibitory activity,have been reported previously.Conclusions Our results show that the methodology used in this study is feasible,credible,and rapid in identifying known compounds and also for characterizing new natural glucosidase inhibitory candidates from Clerodendrum bungei Steud(Chou Mu Dan,臭牡丹). 展开更多
关键词 α-glucosidase inhibitor Clerodendrum bungei Steud(Chou Mu Dan 臭牡丹) hplc-esi-qtof-ms/MS
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HPLC-ESI-QTOF-MS法测定减肥保健食品中16种食欲抑制剂的研究
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作者 宋健 《食品安全导刊》 2020年第27期112-112,共1页
本文提出了以HPLC-ESI-QTOF-MS法测定减肥保健食品中16种食欲抑制剂,以为检测机构提供理论与实践帮助,保障减肥保健食品的健康使用。
关键词 hplc-esi-qtof-ms 减肥保健食品 食欲抑制剂
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HPLC-ESI-QTOF-MS法测定减肥保健食品中16种食欲抑制剂 被引量:5
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作者 孙婷婷 徐彦红 +1 位作者 张雪梅 郑绵冬 《分析试验室》 CAS CSCD 北大核心 2019年第12期1449-1453,共5页
建立高效液相色谱-电喷雾离子化-四级杆串联飞行时间质谱法(HPLC-ESI-QTOF-MS)高通量快速测定减肥保健食品中16种食欲抑制剂的含量。样品经甲醇超声萃取、Oasis MCX固相萃取柱净化,以甲醇和有乙酸铵溶液为流动相,梯度洗脱,采用QTOF-MS... 建立高效液相色谱-电喷雾离子化-四级杆串联飞行时间质谱法(HPLC-ESI-QTOF-MS)高通量快速测定减肥保健食品中16种食欲抑制剂的含量。样品经甲醇超声萃取、Oasis MCX固相萃取柱净化,以甲醇和有乙酸铵溶液为流动相,梯度洗脱,采用QTOF-MS质谱仪进行分析。结果表明:16种食欲抑制剂在1.0~100.0 ng/mL范围内具有良好的线性关系,相关系数≥0.9995;方法检出限在0.03~0.30μg/kg,方法定量限在0.10~1.00μg/kg;加标回收率在91.7%~99.2%,相对标准偏差在1.1%~3.9%。 展开更多
关键词 减肥保健食品 hplc-esi-qtof-ms 食欲抑制剂 非法添加
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大鼠肠道菌群对ilexsaponin A_(1)体外代谢转化的影响
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作者 曹迪 崔辉 赵钟祥 《中成药》 CAS CSCD 北大核心 2023年第1期276-281,共6页
目的考察大鼠肠道菌群对毛冬青三萜皂苷ilexsaponin A_(1)体外代谢转化的影响。方法采用HPLC-ESI-QTOF-MS/MS法检测ilexsaponin A_(1)体外肠道菌孵育样品,条件为Kromasil 100-5 C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相乙腈(含0.1... 目的考察大鼠肠道菌群对毛冬青三萜皂苷ilexsaponin A_(1)体外代谢转化的影响。方法采用HPLC-ESI-QTOF-MS/MS法检测ilexsaponin A_(1)体外肠道菌孵育样品,条件为Kromasil 100-5 C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相乙腈(含0.1%甲酸)-0.1%甲酸,梯度洗脱;体积流量1.0 mL/min;柱温30℃;电喷雾离子源(ESI);负离子模式。对代谢产物进行筛查鉴定,结合二级质谱图,推测代谢产物及其可能的生物转化途径。结果鉴定出14个代谢产物(M1~M14),ilexsaponin A_(1)发生了去糖基化、氧化、还原等代谢反应(M1~M2、M4~M5、M7~M8),其脱糖生成的苷元ilexgenin A进一步发生氧化、羟甲基化、还原等生物转化反应(M3、M6、M9~M11、M13~M14)。结论ilexsaponin A_(1)在大鼠肠道菌群中发生代谢转化,该成分在体内发挥药效并不完全以原型物吸收入血,其苷元ilexgenin A或脱糖后的代谢转化物为其可能的药效物质。 展开更多
关键词 ilexsaponin A_(1) 毛冬青 大鼠肠道菌群 体外代谢转化 hplc-esi-qtof-ms/MS
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桂枝茯苓胶囊HPLC-ESI-QTOF/MS化学成分分析过程中提取溶剂的优化 被引量:6
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作者 李维思 黄玲玲 +2 位作者 李振江 唐美华 郭凯 《生物加工过程》 CAS 2016年第4期59-64,共6页
采用高效液相色谱电喷雾四极杆飞行时间串联质谱(HPLC-ESI-QTOF/MS)对桂枝茯苓胶囊中的化学成分进行分离和鉴别。运用Agilent Eclipse XDB-C18(4.6 mm×250 mm,5μm)色谱柱,以0.1%甲酸水溶液-乙腈为流动相梯度洗脱;使用ESI离子源,... 采用高效液相色谱电喷雾四极杆飞行时间串联质谱(HPLC-ESI-QTOF/MS)对桂枝茯苓胶囊中的化学成分进行分离和鉴别。运用Agilent Eclipse XDB-C18(4.6 mm×250 mm,5μm)色谱柱,以0.1%甲酸水溶液-乙腈为流动相梯度洗脱;使用ESI离子源,正离子与负离子模式下采集数据。根据Q-TOF/MS正、负离子质谱信息、通过元素组成分析、化合物同位素分布验证和对质谱裂解碎片解析并与相关文献对照,鉴别了桂枝茯苓胶囊中18个化合物。本法为桂枝茯苓胶囊中的化学成分分析提供了一种快速、有效的方法。 展开更多
关键词 HPLC-ESI-QTOF/MS 桂枝茯苓胶囊 化学成分 裂解途径
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Structural characterization of monoterpene indole alkaloids in ethanolic extracts of Rauwolfia species by liquid chromatography with quadrupole time-of-flight mass spectrometry 被引量:8
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作者 Sunil Kumar Awantika Singh +3 位作者 Vikas Bajpai Mukesh Srivastava Bhim Pratap Singh Brijesh Kumar 《Journal of Pharmaceutical Analysis》 SCIE CAS 2016年第6期363-373,共11页
Rauwolfia species(Apocynaceae) are medicinal plants well known worldwide due to its potent bioactive monoterpene indole alkaloids(MIAs) such as reserpine,ajmalicine,ajmaline,serpentine and yohimbine.Reserpine,ajmalici... Rauwolfia species(Apocynaceae) are medicinal plants well known worldwide due to its potent bioactive monoterpene indole alkaloids(MIAs) such as reserpine,ajmalicine,ajmaline,serpentine and yohimbine.Reserpine,ajmalicine and ajmaline are powerful antihypertensive,tranquilizing agents used in hypertension.Yohimbine is an aphrodisiac used in dietary supplements.As there is no report on the comparative and comprehensive phytochemical investigation of the roots of Rauwolfia species,we have developed an efficient and reliable liquid chromatography-tandem mass spectrometry(LC–MS/MS) method for ethanolic root extract of Rauwolfia species to elucidate the fragmentation pathways for dereplication of bioactive MIAs using highperformance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry(HPLC–ESI–QTOF–MS/MS) in positive ion mode.We identified and established diagnostic fragment ions and fragmentation pathways using reserpine,ajmalicine,ajmaline,serpentine and yohimbine.The MS/MS spectra of reserpine,ajmalicine,and ajmaline showed C-ring-cleavage whereas E-ring cleavage was observed in serpentine via Retro Diels Alder(RDA).A total of 47 bioactive MIAs were identified and characterized on the basis of their molecular formula,exact mass measurements and MS/MS analysis.Reserpine,ajmalicine,ajmaline,serpentine and yohimbine were unambiguously identified by comparison with their authentic standards and other 42 MIAs were tentatively identified and characterized from the roots of Rauwolfia hookeri,Rauwolfia micrantha,Rauwolfia serpentina,Rauwolfia verticillata,Rauwolfia tetraphylla and Rauwolfia vomitoria.Application of LC–MS followed by principal component analysis(PCA) has been successfully used to discriminate among six Rauwolfia species. 展开更多
关键词 Rauwolfia SPECIES MONOTERPENE INDOLE ALKALOIDS (MIAs) HPLC–ESI–QTOF–MS/MS Principal component analysis (PCA)
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