High-performance thin-layer chromatography-mass spectrometry(HPTLC-MS)is one of the most modern hyphenated analytical methods available today.HPTLC-MS has recently been used to perform extensive analytical work using ...High-performance thin-layer chromatography-mass spectrometry(HPTLC-MS)is one of the most modern hyphenated analytical methods available today.HPTLC-MS has recently been used to perform extensive analytical work using advanced features and still more analyses are in progress using these advanced features.Herbal medicines contain a wide range of bioactives that require proper identification for the activity and quality control.Recently,herbal medicine identification and quality control have become increasingly popular using high-performance liquid chromatography mass spectrometry.The aim of this paper is to provide a brief overview of recent method developments in analysis,15 most significant herbal drug applications with their chromatographic conditions,pharmacological actions,and solvents used in the present paper.An extensive literature search was performed incorporating several databases,notably,Web of Knowledge,PubMed and Google Scholar,and other relevant published materials.In previous research,HPTLC and its hyphenation with MS allowed for quantification of analytes in complex matrixes at nanogram and picogram concentrations.Quantifying a wide variety of analytes using these techniques has been extremely accurate,selective,and sensitive.Throughout this review,the HPTLC-MS technique is discussed in relation to the quality control of herbal drugs.Hence,15 herbal drugs were identified based on their RF values and m/z ratio by mass spectrometry by HPTLC-MS for the first time.In this compilation,researchers can gain insights into HPTLC-MS techniques for resolving quality control issues with herbal drugs using their fingerprint spectra.Besides,the application of HPTLC-MS methods could to be sufficiently precise and reproducible for established conditions and after validation may be used for routine quality control of herbal drugs/formulations in herbal industries.展开更多
Drugs are traditionally been identified on basis of chromatographic-spectroscopic hyphenated techniques in instrumental analysis. Gas chromatography (GC) and Liquid chromatography (LC) hyphenated with mass spectroscop...Drugs are traditionally been identified on basis of chromatographic-spectroscopic hyphenated techniques in instrumental analysis. Gas chromatography (GC) and Liquid chromatography (LC) hyphenated with mass spectroscopy (MS) i.e. GC-MS and LC-MS give reliable and confirmatory results in drugs identification. In the present work the novel hyphenated technique High Performance Thin Layer Chromatography-Mass Spectroscopy (HPTLC-MS) has been used. This technique provides efficient, quick and simple method for identification and separation of Narcotic drugs and psychotropic substances. The drugs under study are Papaverine, Methadone, Cocaine, Ketamine, Caffeine, Codeine, Diazepam, Thebaine, Heroin, Methamphetamine, Carbamazepine, Morphine, Narcotine and Ephedrine. The present study comprising of sixteen drugs has been carried out on CAMAG HPTLC instrument with automatic sampling. Thin layer chromatography (TLC) plates were developed in various solvent systems, scanned under TLC scanner and the results in terms of Retention Factor (Rf value) and UV spectrum (λmax) are presented in the manuscript. Using hyphenated technique of HPTLC-MS (MS 2020 SHIMADZU) spots of these drugs from TLC plate was lifted with CAMAG TLC-MS interface and confirmed by the mass spectrum of the individual drugs by their m/z values thus delivering fast and accurate confirmatory result on the TLC plate.展开更多
母乳中肪酸组成对婴儿后天健康成长具有重要影响。大量测定和发现国人母乳中脂肪酸组成及分布信息不仅有助于制造更适合婴儿需要的母乳代用品,而且有助于指导通过母体补充的方式促进婴儿摄入具有功能特性的脂肪酸。样品经高效薄层色谱分...母乳中肪酸组成对婴儿后天健康成长具有重要影响。大量测定和发现国人母乳中脂肪酸组成及分布信息不仅有助于制造更适合婴儿需要的母乳代用品,而且有助于指导通过母体补充的方式促进婴儿摄入具有功能特性的脂肪酸。样品经高效薄层色谱分离,甲酯化后,以SP2560柱(100 m×0.25 mm ID 0.20μm)分离,四级杆质谱定性定量,建立了高效薄层色谱-气相色谱-四级杆质谱(GC-MS)分析母乳中脂肪酸组成及分布的方法。四级杆质量扫描范围为50~500,扫描速率为20 000 amu/s。方法能够获得母乳中甘油三酯、甘油二酯、甘油磷脂中的脂肪酸组成及总脂肪酸分布,检出限符合方法学要求,为大批量调查国人母乳脂溶性成分的研究奠定技术基础。展开更多
目的构建黄精炮制品多糖的酶水解产物指纹图谱,结合化学计量学方法评价不同蒸晒次数黄精炮制品多糖的差异。方法采用糖苷酶水解,结合高效薄层色谱(high thin-layer chromatography,HPTLC)、亲水作用色谱-高效液相色谱-蒸发光检测器(hydr...目的构建黄精炮制品多糖的酶水解产物指纹图谱,结合化学计量学方法评价不同蒸晒次数黄精炮制品多糖的差异。方法采用糖苷酶水解,结合高效薄层色谱(high thin-layer chromatography,HPTLC)、亲水作用色谱-高效液相色谱-蒸发光检测器(hydrophilic interaction liquid chromatography-high performance liquid chromatography-evaporative light scattering detector,HILIC-HPLC-ELSD)和超高效液相色谱-四级杆飞行时间串联质谱(ultra high pressure liquid chromatographyquadrupole time of flight tandem mass spectrometry,UHPLC-QTOF/MS)对相应的酶解产物进行高效分离和检测。由此产生的自下而上的指纹图谱反映了黄精炮制品多糖的变化,通过相似度和偏最小二乘-判别分析(partial least squares-discriminant analysis,PLS-DA)对指纹图谱进行综合评价。结果HPTLC分析发现,果糖随着蒸晒次数的增加逐渐降低,结合色谱分析发现,六蒸六晒和十二蒸十二晒为黄精炮制过程中的转折点。同时根据酶水解中寡糖的变化,利用相似度和PLS-DA对不同蒸晒次数的黄精炮制品进行了清晰的聚类。结合UHPLC-QTOF/MS分析表明,不同蒸晒次数黄精炮制品中含有蔗糖、蔗果三糖、蔗果四糖、蔗果五糖、蔗果六糖、蔗果七糖及蔗果八糖。结论基于酶解法分析不同蒸晒次数样品的质量动态变化,结合所建立的多元指纹图谱,进一步阐释了不同蒸晒次数黄精炮制品的科学内涵。展开更多
Bioactivity and constituents of 8 common seaweeds from Dalian intertidal zone of northern Yellow Sea were investigated. In the anti-methicillin-resistant Staphylococcus aureus (MRSA) test, Symphyocladia latiuscula and...Bioactivity and constituents of 8 common seaweeds from Dalian intertidal zone of northern Yellow Sea were investigated. In the anti-methicillin-resistant Staphylococcus aureus (MRSA) test, Symphyocladia latiuscula and Enteromorpha intestinalis showed obvious activities with MICs much lower than 1.0 mg·mL-1 . In the DNA damage repair test (DDRT), Chondrus ocellatu showed selective inhibitory activity against the DNA repair-defective E. coli strain vs. the wild-type E. coli strain; while Sym. latiuscula, Enteromorpha intestinalis and Sar. kjellmanianum showed significant anti-E. coli activity with MICs of 64-128 g·mL-1 . In the anti-Pyricularia oryzae test, Sym. latiuscula and Rh. confervoides strongly inhibited the germination of the spores of P. oryzae on agar plate. In the brine shrimp larvicidal test, Sym. latiuscula, Rh. confervoides and Sar. kjellmanianum exhibited potent toxicity against brine shrimp larvae, with LC50 much lower than 1 mg·mL-1 . The HPTLC analysis revealed their diversified secondary metabolites. The HPLC-DAD-MS analysis of the strongest species Sym. latiuscula and database searching showed that it can produce quite diversified metabolites, including halogenated ones, some of which may be new natural products. The results demonstrated the potentials of these seaweeds in the development of new antibiotics, antitumor drugs, agricultural fungicides and pesticides.展开更多
文摘High-performance thin-layer chromatography-mass spectrometry(HPTLC-MS)is one of the most modern hyphenated analytical methods available today.HPTLC-MS has recently been used to perform extensive analytical work using advanced features and still more analyses are in progress using these advanced features.Herbal medicines contain a wide range of bioactives that require proper identification for the activity and quality control.Recently,herbal medicine identification and quality control have become increasingly popular using high-performance liquid chromatography mass spectrometry.The aim of this paper is to provide a brief overview of recent method developments in analysis,15 most significant herbal drug applications with their chromatographic conditions,pharmacological actions,and solvents used in the present paper.An extensive literature search was performed incorporating several databases,notably,Web of Knowledge,PubMed and Google Scholar,and other relevant published materials.In previous research,HPTLC and its hyphenation with MS allowed for quantification of analytes in complex matrixes at nanogram and picogram concentrations.Quantifying a wide variety of analytes using these techniques has been extremely accurate,selective,and sensitive.Throughout this review,the HPTLC-MS technique is discussed in relation to the quality control of herbal drugs.Hence,15 herbal drugs were identified based on their RF values and m/z ratio by mass spectrometry by HPTLC-MS for the first time.In this compilation,researchers can gain insights into HPTLC-MS techniques for resolving quality control issues with herbal drugs using their fingerprint spectra.Besides,the application of HPTLC-MS methods could to be sufficiently precise and reproducible for established conditions and after validation may be used for routine quality control of herbal drugs/formulations in herbal industries.
文摘Drugs are traditionally been identified on basis of chromatographic-spectroscopic hyphenated techniques in instrumental analysis. Gas chromatography (GC) and Liquid chromatography (LC) hyphenated with mass spectroscopy (MS) i.e. GC-MS and LC-MS give reliable and confirmatory results in drugs identification. In the present work the novel hyphenated technique High Performance Thin Layer Chromatography-Mass Spectroscopy (HPTLC-MS) has been used. This technique provides efficient, quick and simple method for identification and separation of Narcotic drugs and psychotropic substances. The drugs under study are Papaverine, Methadone, Cocaine, Ketamine, Caffeine, Codeine, Diazepam, Thebaine, Heroin, Methamphetamine, Carbamazepine, Morphine, Narcotine and Ephedrine. The present study comprising of sixteen drugs has been carried out on CAMAG HPTLC instrument with automatic sampling. Thin layer chromatography (TLC) plates were developed in various solvent systems, scanned under TLC scanner and the results in terms of Retention Factor (Rf value) and UV spectrum (λmax) are presented in the manuscript. Using hyphenated technique of HPTLC-MS (MS 2020 SHIMADZU) spots of these drugs from TLC plate was lifted with CAMAG TLC-MS interface and confirmed by the mass spectrum of the individual drugs by their m/z values thus delivering fast and accurate confirmatory result on the TLC plate.
文摘母乳中肪酸组成对婴儿后天健康成长具有重要影响。大量测定和发现国人母乳中脂肪酸组成及分布信息不仅有助于制造更适合婴儿需要的母乳代用品,而且有助于指导通过母体补充的方式促进婴儿摄入具有功能特性的脂肪酸。样品经高效薄层色谱分离,甲酯化后,以SP2560柱(100 m×0.25 mm ID 0.20μm)分离,四级杆质谱定性定量,建立了高效薄层色谱-气相色谱-四级杆质谱(GC-MS)分析母乳中脂肪酸组成及分布的方法。四级杆质量扫描范围为50~500,扫描速率为20 000 amu/s。方法能够获得母乳中甘油三酯、甘油二酯、甘油磷脂中的脂肪酸组成及总脂肪酸分布,检出限符合方法学要求,为大批量调查国人母乳脂溶性成分的研究奠定技术基础。
文摘目的构建黄精炮制品多糖的酶水解产物指纹图谱,结合化学计量学方法评价不同蒸晒次数黄精炮制品多糖的差异。方法采用糖苷酶水解,结合高效薄层色谱(high thin-layer chromatography,HPTLC)、亲水作用色谱-高效液相色谱-蒸发光检测器(hydrophilic interaction liquid chromatography-high performance liquid chromatography-evaporative light scattering detector,HILIC-HPLC-ELSD)和超高效液相色谱-四级杆飞行时间串联质谱(ultra high pressure liquid chromatographyquadrupole time of flight tandem mass spectrometry,UHPLC-QTOF/MS)对相应的酶解产物进行高效分离和检测。由此产生的自下而上的指纹图谱反映了黄精炮制品多糖的变化,通过相似度和偏最小二乘-判别分析(partial least squares-discriminant analysis,PLS-DA)对指纹图谱进行综合评价。结果HPTLC分析发现,果糖随着蒸晒次数的增加逐渐降低,结合色谱分析发现,六蒸六晒和十二蒸十二晒为黄精炮制过程中的转折点。同时根据酶水解中寡糖的变化,利用相似度和PLS-DA对不同蒸晒次数的黄精炮制品进行了清晰的聚类。结合UHPLC-QTOF/MS分析表明,不同蒸晒次数黄精炮制品中含有蔗糖、蔗果三糖、蔗果四糖、蔗果五糖、蔗果六糖、蔗果七糖及蔗果八糖。结论基于酶解法分析不同蒸晒次数样品的质量动态变化,结合所建立的多元指纹图谱,进一步阐释了不同蒸晒次数黄精炮制品的科学内涵。
基金supported by the National Natural Science Foundation of China (20902009)Postdoctoral Science Foundation of China (2011M-500051 and 2012T50242)+1 种基金the Key Laboratory of Experimental Marine Biology, Institute of Oceanology, Chinese Academy of Sciences (kf201009)the Scientific and Technological Fund of Dalian (2008J23JH041)
文摘Bioactivity and constituents of 8 common seaweeds from Dalian intertidal zone of northern Yellow Sea were investigated. In the anti-methicillin-resistant Staphylococcus aureus (MRSA) test, Symphyocladia latiuscula and Enteromorpha intestinalis showed obvious activities with MICs much lower than 1.0 mg·mL-1 . In the DNA damage repair test (DDRT), Chondrus ocellatu showed selective inhibitory activity against the DNA repair-defective E. coli strain vs. the wild-type E. coli strain; while Sym. latiuscula, Enteromorpha intestinalis and Sar. kjellmanianum showed significant anti-E. coli activity with MICs of 64-128 g·mL-1 . In the anti-Pyricularia oryzae test, Sym. latiuscula and Rh. confervoides strongly inhibited the germination of the spores of P. oryzae on agar plate. In the brine shrimp larvicidal test, Sym. latiuscula, Rh. confervoides and Sar. kjellmanianum exhibited potent toxicity against brine shrimp larvae, with LC50 much lower than 1 mg·mL-1 . The HPTLC analysis revealed their diversified secondary metabolites. The HPLC-DAD-MS analysis of the strongest species Sym. latiuscula and database searching showed that it can produce quite diversified metabolites, including halogenated ones, some of which may be new natural products. The results demonstrated the potentials of these seaweeds in the development of new antibiotics, antitumor drugs, agricultural fungicides and pesticides.