Gumiganghwal-tang is a traditional herbal medicine widely used for its anti-inflammatory,analgesic,and antipyretic effects.However,the safety and efficacy of its active ingredients based on an in vivo pharmacokinetic(...Gumiganghwal-tang is a traditional herbal medicine widely used for its anti-inflammatory,analgesic,and antipyretic effects.However,the safety and efficacy of its active ingredients based on an in vivo pharmacokinetic(PK)study have yet been investigated.We have established a sensitive and accurate UPLC-ESI-MS/MS method and conducted a PK study on 14 constituents of Gumiganghwal-tang through human plasma analysis.Analytical conditions were optimized according to the physicochemical properties of the 14 compounds to facilitate efficient separation and eliminate overlap or interference between peaks.KINETEX-C18 and Inertsil-C8 columns were used as UPLC stationary phases,and acetonitrile and aqueous formic acid were used as mobile phases.All the analytes were quantified with a triple quadrupole mass spectrometer using electrospray ionization in multiple reaction monitoring mode.The chromatograms of 14 bioactive compounds showed excellent elution and sensitivity,and each peak was selectively separated and quantified without interference with each other or impurities.The established analytical method was based on international guidelines and was successfully used to perform PK studies of 14 herbal ingredients in humans after oral administration with Gumiganghwal-tang tablets.The oral absorption of most active components of Gumiganghwal-tang was relatively rapid and remained considerably long in the body to be quantified in plasma up to 48 h after administration.展开更多
Alkaloids are nitrogen-containing organic compounds, generally basic, and found in plants, fungi, and bacteria. Some alkaloids are used in medicine, but some compounds are highly toxic. Accidental ingestion, homicide,...Alkaloids are nitrogen-containing organic compounds, generally basic, and found in plants, fungi, and bacteria. Some alkaloids are used in medicine, but some compounds are highly toxic. Accidental ingestion, homicide, and suicide have occurred due to plants containing alkaloids. The identification of toxic components in biological samples is important for the diagnosis and/or treatment of poisoning cases in forensic and emergency medicine. Alkaloids have a wide variety of structures, such as isoquinoline alkaloid, indole alkaloid, tropane alkaloid, and diterpene alkaloid;therefore, there are few reports of simultaneous analysis methods. We have established a method for the simultaneous analysis of 23 alkaloids in human serum with a liquid chromatograph-tandem mass spectrometer (LC/MS/MS). A liquid-liquid extraction which was modified from the first step of the QuEChERS AOAC method was used for serum pretreatment. The separation of the compounds was performed using a pentafluorophenyl (PFP) column, CAPCELL CORE PFP (2.1 mm I.D. × 100 mm, 2.7 μm) in gradient mode. Mobile phase A consisted of 10 mM ammonium formate and 0.1% formic acid in ultrapure water, and mobile phase B was 10 mM ammonium formate and 0.1% formic acid in methanol. Simultaneous analysis was performed in dynamic multiple reaction monitoring mode. The separation of 23 alkaloids was satisfactory, as PFP columns exhibited different retention behaviors than alkyl phase columns. The PFP column effectively retained polar aromatic compounds;therefore, it was suitable for alkaloid analysis. The validated method was applied to a forensic case of aconite poisoning. The present method was useful in LC/MS/MS screening for 23 alkaloids in human serum.展开更多
AIM: To develop a high performance liquid chromatography(HPLC) coupled with electrospray ionization mass spectrometry(ESI-MS) and ultraviolet(UV) detector method for the acid-alkaline simultaneous determination of ten...AIM: To develop a high performance liquid chromatography(HPLC) coupled with electrospray ionization mass spectrometry(ESI-MS) and ultraviolet(UV) detector method for the acid-alkaline simultaneous determination of ten bioactive compounds, and analyze the effect of compatible medicinal plants on the concentration of components in Dahuang Fuzi Tang(DFT). METHOD: The chromatographic separation was performed on a Hypersil BDS C18 analytical column by gradient elution with acetonitrile and formate buffer(containing 0.15% formic acid, V/V) at 25 °C with a flow rate of 1.0 mL ·min–1 and UV detection at 280 nm. Four of the ten compounds in DFT were identified and their MS fragments were elucidated by HPLC-ESI-MS, and the contents of the six compounds were determined by HPLC-UV. RESULTS: All calibration curves showed good linear regression(r2 ≥ 0.9990). The limits of detection and limits of quantification were 0.021–0.155 μg·mL –1 and 0.076–0.520 μg·mL –1, respectively. Overall precision RSD(intra-day and inter-day) were less than 2.96%, and the average recoveries were 98.35%–101.45%, with RSD ranging from 1.54% to 3.01% for the analytes. CONCLUSION: The developed method can be applied for the quality control and provide analytical evidence on the chemical basis and combinational principles of DFT.展开更多
基金supported by a grant from the National Development Institute of Korean Medicine(NIKOM)funded by the Korean Ministry of Health and Welfare(MOHW),Republic of Korea。
文摘Gumiganghwal-tang is a traditional herbal medicine widely used for its anti-inflammatory,analgesic,and antipyretic effects.However,the safety and efficacy of its active ingredients based on an in vivo pharmacokinetic(PK)study have yet been investigated.We have established a sensitive and accurate UPLC-ESI-MS/MS method and conducted a PK study on 14 constituents of Gumiganghwal-tang through human plasma analysis.Analytical conditions were optimized according to the physicochemical properties of the 14 compounds to facilitate efficient separation and eliminate overlap or interference between peaks.KINETEX-C18 and Inertsil-C8 columns were used as UPLC stationary phases,and acetonitrile and aqueous formic acid were used as mobile phases.All the analytes were quantified with a triple quadrupole mass spectrometer using electrospray ionization in multiple reaction monitoring mode.The chromatograms of 14 bioactive compounds showed excellent elution and sensitivity,and each peak was selectively separated and quantified without interference with each other or impurities.The established analytical method was based on international guidelines and was successfully used to perform PK studies of 14 herbal ingredients in humans after oral administration with Gumiganghwal-tang tablets.The oral absorption of most active components of Gumiganghwal-tang was relatively rapid and remained considerably long in the body to be quantified in plasma up to 48 h after administration.
文摘Alkaloids are nitrogen-containing organic compounds, generally basic, and found in plants, fungi, and bacteria. Some alkaloids are used in medicine, but some compounds are highly toxic. Accidental ingestion, homicide, and suicide have occurred due to plants containing alkaloids. The identification of toxic components in biological samples is important for the diagnosis and/or treatment of poisoning cases in forensic and emergency medicine. Alkaloids have a wide variety of structures, such as isoquinoline alkaloid, indole alkaloid, tropane alkaloid, and diterpene alkaloid;therefore, there are few reports of simultaneous analysis methods. We have established a method for the simultaneous analysis of 23 alkaloids in human serum with a liquid chromatograph-tandem mass spectrometer (LC/MS/MS). A liquid-liquid extraction which was modified from the first step of the QuEChERS AOAC method was used for serum pretreatment. The separation of the compounds was performed using a pentafluorophenyl (PFP) column, CAPCELL CORE PFP (2.1 mm I.D. × 100 mm, 2.7 μm) in gradient mode. Mobile phase A consisted of 10 mM ammonium formate and 0.1% formic acid in ultrapure water, and mobile phase B was 10 mM ammonium formate and 0.1% formic acid in methanol. Simultaneous analysis was performed in dynamic multiple reaction monitoring mode. The separation of 23 alkaloids was satisfactory, as PFP columns exhibited different retention behaviors than alkyl phase columns. The PFP column effectively retained polar aromatic compounds;therefore, it was suitable for alkaloid analysis. The validated method was applied to a forensic case of aconite poisoning. The present method was useful in LC/MS/MS screening for 23 alkaloids in human serum.
基金financially supported by the National Natural Science Foundation of China(No.81073022)
文摘AIM: To develop a high performance liquid chromatography(HPLC) coupled with electrospray ionization mass spectrometry(ESI-MS) and ultraviolet(UV) detector method for the acid-alkaline simultaneous determination of ten bioactive compounds, and analyze the effect of compatible medicinal plants on the concentration of components in Dahuang Fuzi Tang(DFT). METHOD: The chromatographic separation was performed on a Hypersil BDS C18 analytical column by gradient elution with acetonitrile and formate buffer(containing 0.15% formic acid, V/V) at 25 °C with a flow rate of 1.0 mL ·min–1 and UV detection at 280 nm. Four of the ten compounds in DFT were identified and their MS fragments were elucidated by HPLC-ESI-MS, and the contents of the six compounds were determined by HPLC-UV. RESULTS: All calibration curves showed good linear regression(r2 ≥ 0.9990). The limits of detection and limits of quantification were 0.021–0.155 μg·mL –1 and 0.076–0.520 μg·mL –1, respectively. Overall precision RSD(intra-day and inter-day) were less than 2.96%, and the average recoveries were 98.35%–101.45%, with RSD ranging from 1.54% to 3.01% for the analytes. CONCLUSION: The developed method can be applied for the quality control and provide analytical evidence on the chemical basis and combinational principles of DFT.
