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Diagnostic ion filtering to characterize ginseng saponins by rapid liquidchromatography with time-of-flight mass spectrometry

Diagnostic ion filtering to characterize ginseng saponins by...

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中华中医药学会中药分析分会第五届学术交流会

作者： LianWen Qi HuaiYou Wang Hui Zhang ChongZhi Wang Ping Li ChunSu Yuan

As one of the most commonly used medicinal plants,ginseng has been an attractive model herb for study.A wide range of analytical methods has been used to characterize its ***,less effort has been devoted to the rare ginseng saponins,especially their isomers and sugar *** this study,we used segmental monitoring and diagnostic ion filtering to characterize ginseng saponins by rapid liquid chromatography with time-of-flight mass spectrometry (LC-TOF-MS).By using selected diagnostic ions,specific groups of ginseng saponins were readily extracted from the complicated matrix.20? and 20(S) stereo-saponins were differentiated using the peak abundance ratio of [M-H2O+H]+ to [M-2H2O+H]+.The fragmentation behavior of ginsenosides was first reported in negative ion mode by MS/MS with high-energy collision-induced dissociation,producing rules to determine sugar numbers,positions and *** the rules,we identified and compared the nontarget ginseng saponin profiling of raw and steamed American ginseng roots and *** characterized 70 saponins in the *** strategy can be extended to screen and characterize other rare ginseng saponins and their metabolites

关键词： Ginseng Ginseng saponins Ginsenosides Liquid chromatography time-of-flight mass spectrometry Segmental monitoring Diagnostic ion filtering

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Simultaneous determination of triterpenoid saponins in dog plasma by a validated UPLC-MS/MS and its application to a pharmacokinetic study after administration of licorice total saponins

Simultaneous determination of triterpenoid saponins in dog p...

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中华中医药学会中药分析分会第五届学术交流会

作者： Weiwei Tao~(a,b),Jinao Duan~(a,b),Jianming Guo~a,Yuping Tang~a,Pei Liu~a,Nianyun Yang~a, Jianping Li~a a Jiangsu Key Laboratory for High Technology Research of TCM Formulae,Nanjing University of Chinese Medicine,Nanjing 210046, China b School of Traditional Chinese Medicine,China Pharmaceutical University,Nanjing

A rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for simultaneous determination of nine active constituents,uralsaponin C, uralsaponin F,22-acetoxyl-glycyrrhizin,24-hydroxy-licorice-saponin E2,licorice-saponin G2,licorice-saponin E2, 22-acetoxyl-glycyrrhaldehyde,glycyrrhizin,and licorice-saponin J2,from licorice total saponins(LTS) in dog *** A was used as the internal standard(IS).The separation was performed on Thermo Syncronic C18 column(100mm×2.1 mm,1.7μm) at a flow rate of 0.4 mL min-1,and acetonitrile-0.1%formic acid was used as mobile *** detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring(MRM) via electrospray ionization(ESI) source with negative ionization *** calibration curves have good linearity(r > 0.991) over the concentration range from 2.03 - 405 ng/mL to 2.63 - 2625 ng/mL for all *** intra- and inter-day precision(RSD%) was within 15%and the accuracy ranged from 85.92%to 113.8%.The method was successfully applied to pharmacokinetic study of nine triterpenoid saponins in dog plasma after oral administration of LTS.

关键词： Simultaneous determination of triterpenoid saponins in dog plasma by a validated UPLC-MS/MS and its application to a pharmacokinetic study after administration of licorice total saponins

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Rapid determination of amino acids without derivatization using hydrophilic interaction ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry

Rapid determination of amino acids without derivatization us...

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中华中医药学会中药分析分会第五届学术交流会

作者： Sheng Guo,Jin-ao Duan~*,Dawei Qian,Yuping Tang,Yefei Qian,Dawei Wu,Shulan Su,Erxin Shang Jiangsu Key Laboratory for High Technology Research of TCM Formulae,Nanjing University of Chinese Medicine,Nanjing 210046,PR. China

A novel hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry （HIL1C-MS/MS） method was developed for the simultaneous determination of 23 free amino acids without *** method was performed on an ultra-high performance liquid chromatography（UHPLC） separation system coupled with electrospray ionization mass spectrometry on a triple quadrupole mass spectrometer （TQ-MS）,operating in positive ionization *** separation of the 23 underivatized amino acids was achieved on an Acquity BEH Amide column（2.1 mm×100 mm,1.7μm） in a single run of 12 min at a flow rate of 0.4 mL *** limits of detection were in the range from 0.17 to 77.75 ng *** the analytes were quantified directly from biological extracts without any kind of derivatization,which avoided the laborious and time-consuming of derivatization procedures used by the traditional ***,the more polar compounds were separated without utilization of perfluorinated acids as ion-pairing reagents which was not suggested for ESI source. Then,the method was applied for the analysis of the free amino acids in 46 batches of Ziziphus jujuba fruits which comprised 39 cultivars from 26 cultivation *** statistical analysis was also used to investigate the differences in free amino acid profiles among the *** study showed that HILIC-UHPLC-TQ-MS is an effective technique to analyze underivatized amino acids in the biological samples.

关键词： Amino acid Ziziphus jujuba Hydrophilic interaction chromatography Ultra-high performance liquid chromatography Triple quadrupole mass spectrometry

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Simultaneous determination of triterpenoid saponins in dog plasma by a validated UPLC-MS/MS and its application to a pharmacokinetic study after administration of licorice total saponins

Simultaneous determination of triterpenoid saponins in dog p...

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中华中医药学会中药分析分会第五届学术交流会

作者： Weiwei Tao Jinao Duan Jianming Guo Yuping Tang Pei Liu Nianyun Yang Jianping Li Jiangsu Key Laboratory for High Technology Research of TCM Formulae Nanjing University of Chinese Me Jiangsu Key Laboratory for High Technology Research of TCM Formulae Nanjing University of Chinese Me

A rapid and sensitive ultra performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed for simultaneous determination of nine active constituents,uralsaponin C,uralsaponin F,22-acetoxyl-glycyrrhizin,24-hydroxy-licorice-saponin E2,licorice-saponin G2,licorice-saponin E2,22-acetoxyl-glycyrrhaldehyde,glycyrrhizin,and licorice-saponin J2,from licorice total saponins (LTS) in dog *** A was used as the internal standard (IS).The separation was performed on Thermo Syncronic C18 column (100 mm×2.1 mm,1.7 μm) at a flow rate of 0.4 mL min?1,and acetonitrile-0.1% formic acid was used as mobile *** detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) via electrospray ionization (ESI) source with negative ionization *** calibration curves have good linearity (r > 0.991) over the concentration range from 2.03 – 405 ng/mL to 2.63 – 2625 ng/mL for all *** intra- and inter-day precision (RSD %) was within 15% and the accuracy ranged from 85.92 % to 113.8%.The method was successfully applied to pharmacokinetic study of nine triterpenoid saponins in dog plasma after oral administration of LTS.

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Rapid determination of amino acids without derivatization using hydrophilic interaction ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry

Rapid determination of amino acids without derivatization us...

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中华中医药学会中药分析分会第五届学术交流会

作者： Sheng Guo Jinao Duan Dawei Qian Yuping Tang Yefei Qian Dawei Wu Shulan Su Erxin Shang Jiangsu Key Laboratory for High Technology Research of TCM Formulae Nanjing University of Chinese MedicineNanjing 210046P.R. China

A novel hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry (HILIC-MS/MS) method was developed for the simultaneous determination of 23 free amino acids without *** method was performed on an ultra-high performance liquid chromatography (UHPLC) separation system coupled with electrospray ionization mass spectrometry on a triple quadrupole mass spectrometer (TQ-MS),operating in positive ionization *** separation of the 23 underivatized amino acids was achieved on an Acquity BEH Amide column (2.1 mm × 100 mm,1.7 um) in a single run of 12 min at a flow rate of 0.4 mL *** limits of detection were in the range from 0.17 to 77.75 ng *** the analytes were quantified directly from biological extracts without any kind of derivatization,which avoided the laborious and time-consuming of derivatization procedures used by the traditional ***,the more polar compounds were separated without utilization of perfluorinated acids as ion-pairing reagents which was not suggested for ESI ***,the method was applied for the analysis of the free amino acids in 46 batches of Ziziphus jujuba fruits which comprised 39 cultivars from 26 cultivation *** statistical analysis was also used to investigate the differences in free amino acid profiles among the *** study showed that HILIC-UHPLC-TQ-MS is an effective technique to analyze underivatized amino acids in the biological samples.

关键词： Amino acid Ziziphus jujuba Hydrophilic interaction chromatography Ultra-high performance liquid chromatography Triple quadrupole mass spectrometry

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Simultaneous determination of 15 nucleosides and nucleobases in natural Cordyceps by hydrophilic interaction chromatography- electrospray ionization tandem mass spectrometry

Simultaneous determination of 15 nucleosides and nucleobases...

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中华中医药学会中药分析分会第五届学术交流会

作者： Xiao Wang~(1,2),Hengqiang Zhao~1,Hongmei Li~2,Bin Yang~2,Hongjun Yang~2,Luqi Huang~(2*) (1 Shandong Analysis and Test Center,Shandong Academy of Sciences,Jinan 250014,China 2 Institute of Chinese Material Medical,China Academy of Chinese Medical Sciences,16 Dongzhimennei Street,Beijing 100700, China)

Cordyceps sinensis has been widely used as traditional Chinese medicines（TCM） in *** date,nucleosides are believed to be the bioactive components in ***,a specific and sensitive analysis method of these compounds is essential for the quality control of *** interaction liquid chromatography（HILIC） was proposed for the separation of highly hydrophilic compounds by Alpert in 1990,which was characterized by polar stationary phases and aqueous-organic mobile *** mass spectrometry could provides low limits of detection and high selectivity capabilities, so the HILIC-ESI-MS/MS method would be more suitable for the quantitative analysis of high polar compound in complex *** this study,a hydrophilic interaction chromatography（HILIC） and electrospray ionization tandem mass spectrometry（ESI -MS/MS） method was developed for the identification and quantification of 15 nucleosides and nucleobases namely thymine,uracil, thymidine,2'-deoxyuridine,cordycepin,uridine,hypoxanthine,adenine,adenosine,xanthine,inosine,cytosine,guanine, cytidine,guanosine in natural *** separation was achieved on a Waters Xbridge Amide column（250x4.6 mm I.D.,3.5 um） and gradient elution using a solution of acetonitrile and buffer（0.20%acetic acid and 10 mmol/L ammonium acetate） as the mobile phase at a flow rate of 0.8 mL/*** of the 16 target nucleosides and nucleobases was based on retention time, UV spectra,mass measurements of the protonated molecules（[M+H]） and main fragment ions（ESI-MS/MS）.Quantitative analysis of investigated compounds were performed using time programmed selective ion monitoring（SIM） or multiple reaction monitoring （MRM） in positive ion mode under optimized mass *** calibration curves showed good linearity（r > 0.9951） within the test *** overall intra- and inter-day RSD ranged from 2.45 to 5.23%and from 3.29 to 6.73%,*** LOD were in the range of 0.15-10.00 ng/mL,respective

关键词： Cordyceps nucleosides and nucleobases hydrophilic interaction chromatography electrospray ionization tandem mass spectrometry

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Rapid characterization of 70 polymethoxylated flavonoids(PMFs) in the leaves of Murraya paniculata *** on-line HPLC-DAD-ESI-MS/MS

Rapid characterization of 70 polymethoxylated flavonoids(PMF...

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中华中医药学会中药分析分会第五届学术交流会

作者： Jia-Yu Zhang~(1,2),Qian Zhang~1,Li-Ping Ye~1,Hong-Xia Zhang~1,Jian-Qiu Lu~(2*),Yan-Jiang Qiao~(1*) 1 School of Chinese Pharmacy,Beijing University of Chinese Medicine,Beijing 100102,China 2 Center of Scientific Experiment,Beijing University of Chinese Medicine,Beijing 100029,China

A sensitive HPLC-DAD-ESI-MS/MS method was established to screen and identify the polymethoxylated flavonoids（PMFs） from the leaves of Murraya paniculata（L.） Jack.15 PMFs references were first analyzed in a positive mode by the CID-MS/*** polymethoxylated flavones,the fragments of [M+H-n×15] produced by loss of one or more methyl groups from the protonated molecule,as well as[M+H-14], [M+H-16],[M+H-28],[M+H-29],[M+H-31],[M+H-33],[M+H-43],[M+H-44],[M+H-46] and [M+H-61] fragment ions were detected,which could be taken as their diagnostic *** polymethoxylated flavanones and chalcones,their[M+H] ions usually underwent RDA cleavage fragmentation of the C-ring prior to the similar loss of diagnostic fragment ions as polymethoxylated flavones,which could be adopted as a shortcut to distinguish them from ordinary flavones *** the PMFs glycosides,besides the neutral loss of the similar fragments as polymethoxylated flavones from their[Aglycone+H],the intensity ratio of [Aglycone+H] to[Aglycone] maintaining at about 5:1 could be used as a simple method to screen them out from a complex *** on these characterizations of PMFs and the results of EIC-MS/MS experiment,70 PMFs including 45 flavones,17 flavanones or chalcones and 8 PMF glycosides were screened from the complex extract of the leaves of Murraya *** results indicated that the developed analysis method could be employed as a rapid and effective technique for the screen and structural characterization of PMFs.

关键词： HPLC-DAD-ESI-MS/MS polymethoxylated flavonoids(PMFs) fragmentation characteristic Murraya paniculata

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Rapid characterization of 70 polymethoxylated flavonoids (PMFs) in the leaves of Murraya paniculata *** on-line HPLC-DAD-ESI-MS/MS

Rapid characterization of 70 polymethoxylated flavonoids (PM...

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中华中医药学会中药分析分会第五届学术交流会

作者： JiaYu Zhang Qian Zhang LiPing Ye HongXia Zhang JianQiu Lu YanJiang Qiao School of Chinese Pharmacy Beijing University of Chinese MedicineBeijing 100102China Center of Sci School of Chinese Pharmacy Beijing University of Chinese MedicineBeijing 100102China Center of Scientific Experiment Beijing University of Chinese MedicineBeijing 100029China

A sensitive HPLC-DAD-ESI-MS/MS method was established to screen and identify the polymethoxylated flavonoids (PMFs) from the leaves of Murraya paniculata (L.) Jack.15 PMFs references were first analyzed in a positive mode by the CID-MS/*** polymethoxylated flavones,the fragments of [M+H-n×15]+ produced by loss of one or more methyl groups from the protonated molecule,as well as [M+H-14]+,[M+H-16]+,[M+H-28]+,[M+H-29]+,[M+H-31]+,[M+H-33]+,[M+H-43]+,[M+H-44]+,[M+H-46]+ and [M+H-61]+ fragment ions were detected,which could be taken as their diagnostic *** polymethoxylated flavanones and chalcones,their [M+H]+ ions usually underwent RDA cleavage fragmentation of the C-ring prior to the similar loss of diagnostic fragment ions as polymethoxylated flavones,which could be adopted as a shortcut to distinguish them from ordinary flavones *** the PMFs glycosides,besides the neutral loss of the similar fragments as polymethoxylated flavones from their [Aglycone+H]+,the intensity ratio of [Aglycone+H]+ to [Aglycone]+? maintaining at about 5:1 could be used as a simple method to screen them out from a complex *** on these characterizations of PMFs and the results of EIC-MS/MS experiment,70 PMFs including 45 flavones,17 flavanones or chalcones and 8 PMF glycosides were screened from the complex extract of the leaves of Murraya *** results indicated that the developed analysis method could be employed as a rapid and effective technique for the screen and structural characterization of PMFs.

关键词： HPLC-DAD-ESI-MS/MS polymethoxylated flavonoids (PMFs) fragmentation characteristic Murraya paniculata

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Pharmacokinetics study of three aromatic acids following oral administration of Shaofu Zhuyu decoction to normal and dysmenorrhea rats

Pharmacokinetics study of three aromatic acids following ora...

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中华中医药学会中药分析分会第五届学术交流会

作者： Shulan Su,Wenxia Cui,Yongqing Hua,Jinao Duan~*,Jianming Guo,Erxin Shang,Xinyue Jing,Pei Liu,Li Liu,Zhenhua Zhu,Yuping Tang Jiangsu Key Laboralory for TCM Formulae Research,Nanjing University of Chinese Medicine,Nanjing 210046,PR China

Shaofu Zhuyu decoction,a famous effective traditional Chinese formula,is commonly utilized for treating blood stasis syndrome of gynecology diseases in clinic for a long *** this paper,we compared the pharmacokinetics profile of three active aromatic acids in normal and dysmenorrhea rats plasma following oral administration of SFZYD and its ethanol supernatant. The rats were randomly divided to six groups and given the same dose of 2.1 mg/kg SFZYD and *** samples were collected at different time(0,0.083,0.25,0.5,1,2,4,6,8,12,24 h) after administration,the concentration of three aromatic acid components were then determined by ultra-performance liquid chromatography/time-of-flight mass spectrometry(UHPLC-QTOF/MS) and main pharmacokinetic parameters were estimated by DAS 2.0 *** aromatic acids were absorbed better in SFZYD than SFE, which was prepared of same amount of crude *** group has a better absorption than normal group which was benefit for therapy efficacy.

关键词： Shaofu Zhuyu decoction Aromatic acids Pharmacokinetics UHPLC-QTOF/MS

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Simultaneous determination of 15 nucleosides and nucleobases in natural Cordyceps by hydrophilic interaction chromatography- electrospray ionization tandem mass spectrometry

Simultaneous determination of 15 nucleosides and nucleobases...

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中华中医药学会中药分析分会第五届学术交流会

作者： Xiao Wang Hengqiang Zhao Hongmei Li Bin Yang Hongjun Yang Luqi Huang Shandong Analysis and Test Center Shandong Academy of SciencesJinan 250014China Institute of Chine Shandong Analysis and Test Center Shandong Academy of SciencesJinan 250014China Institute of Chinese Material Medical China Academy of Chinese Medical Sciences16 Dongzhimennei Str

Cordyceps sinensis has been widely used as traditional Chinese medicines (TCM) in *** date,nucleosides are believed to be the bioactive components in ***,a specific and sensitive analysis method of these compounds is essential for the quality control of *** interaction liquid chromatography (HILIC) was proposed for the separation of highly hydrophilic compounds by Alpert in 1990,which was characterized by polar stationary phases and aqueous-organic mobile *** mass spectrometry could provides low limits of detection and high selectivity capabilities,so the HILIC-ESI-MS/MS method would be more suitable for the quantitative analysis of high polar compound in complex *** this study,a hydrophilic interaction chromatography (HILIC) and electrospray ionization tandem mass spectrometry (ESI-MS/MS) method was developed for the identification and quantification of 15 nucleosides and nucleobases namely thymine,uracil,thymidine,2'-deoxyuridine,cordycepin,uridine,hypoxanthine,adenine,adenosine,xanthine,inosine,cytosine,guanine,cytidine,guanosine in natural *** separation was achieved on a Waters Xbridge Amide column (250×4.6 mm I.D.,3.5 μm) and gradient elution using a solution of acetonitrile and buffer (0.20% acetic acid and 10 mmol/L ammonium acetate) as the mobile phase at a flow rate of 0.8 mL/*** of the 16 target nucleosides and nucleobases was based on retention time,UV spectra,mass measurements of the protonated molecules ([M+H]+) and main fragment ions (ESI-MS/MS).Quantitative analysis of investigated compounds were performed using time programmed selective ion monitoring (SIM) or multiple reaction monitoring (MRM) in positive ion mode under optimized mass *** calibration curves showed good linearity (r2 > 0.9951) within the test *** overall intra- and inter-day RSD ranged from 2.45 to 5.23% and from 3.29 to 6.73%,*** LOD were in the range of 0.15-10.00 ng/mL,r

关键词： Cordyceps nucleosides and nucleobases hydrophilic interaction chromatography electrospray ionization tandem mass spectrometry

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