The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Gi...The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy.展开更多
A sensitive and selective liquid chromatography-electrospray ionization tandem mass spectrometry（LC- ES1-MS/MS） was used for the simultaneous determination of metformin and glimepiride in beagle dog plasma with glip...A sensitive and selective liquid chromatography-electrospray ionization tandem mass spectrometry（LC- ES1-MS/MS） was used for the simultaneous determination of metformin and glimepiride in beagle dog plasma with glipizide as internal standard（IS）. After simplified protein precipitation with methanol, both the analytes and IS were chromatographed on a Zorbax CN column via gradient elution with methanol（containing 5 mmol/L ammonium ace- tate） and 5 mmol/L aqueous ammonium acetate as the mobile phase. Detection was performed by multiple reaction monitoring（MRM） scanning via ESI source operated in positive ionization mode. Specificity, linearity, accuracy, pre- cision, recovery, matrix effect and stability were validated for metformin and glimepiride in beagle dog plasma. The calibration curves were linear in a concentration range of 10-10000 ng/mL for metformin and 4-4000 ng/mL for glimepiride with both correlation coefficients higher than 0.99. The recoveries obtained for the analytes and IS were all between 82.7% and 101.2%. The method exhibited excellent performance in terms of selectivity, robustness, short analytical time and simplicity of sample preparation. Finally, the proposed method was applied to a bioequivalence study of self-made bilayer tablet and commercial formulation containing 500 mg of metformin and 1 mg of glimepi- ride in beagle dogs.展开更多
In this paper, a sensitive and specific liquid chromatography-electrospray ionisation-mass spectrometry （LC-ESI-MS） method has been developed and validated for the identification and determination of seven flavonoid...In this paper, a sensitive and specific liquid chromatography-electrospray ionisation-mass spectrometry （LC-ESI-MS） method has been developed and validated for the identification and determination of seven flavonoids, namely epimedin A, epimedin B, epimedin C, icariin, sagittatoside B, 2＂-O-rhamnosyl icariside II, and baohuoside I in Epimedium from different sources.展开更多
Liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS)is a widely utilized technique for in vivo pharmaceutical analysis.Ionization interference within electrospray ion source,occurring betw...Liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS)is a widely utilized technique for in vivo pharmaceutical analysis.Ionization interference within electrospray ion source,occurring between drugs and metabolites,can lead to signal variations,potentially compromising quantitative accuracy.Currently,method validation often overlooks this type of signal interference,which may result in systematic errors in quantitative results without matrix-matched calibration.In this study,we conducted an investigation using ten different groups of drugs and their corresponding metabolites across three LC-ESI-MS systems to assess the prevalence of signal interference.Such interferences can potentially cause or enhance nonlinearity in the calibration curves of drugs and metabolites,thereby altering the relationship between analyte response and concentration for quantification.Finally,we established an evaluation scheme through a step-by-step dilution assay and employed three resolution methods:chromatographic separation,dilution,and stable labeled isotope internal standards correction.The above strategies were integrated into the method establishment process to improve quantitative accuracy.展开更多
A rapid and sensitive liquid chromatography tandem mass spectrometry(LC-MS/MS) method has been developed and validated for the determination of moxifloxacin(MOXI) in human plasma. After a simple protein precipitation ...A rapid and sensitive liquid chromatography tandem mass spectrometry(LC-MS/MS) method has been developed and validated for the determination of moxifloxacin(MOXI) in human plasma. After a simple protein precipitation using acetonitrile, the post treatment samples were analysed on a C18 column interfaced with a Triple Quadropole Tandem Mass Spectrometer. Positive electrospray ionization was employed as the ionization source. The mobile phase consisted of 0.1% formic acid–acetonitrile(60:40, v/v). Ciprofloxacin(CIPRO) was used as an internal standard. The analyte and internal standard(CIPRO) were monitored in the multiple reaction monitoring mode(MRM). The mass transition ion-pair has been followed as m/z 402→358.2 for MOXI and 332→288.1 for CIPRO. The method was linear in the concentration range of 25–5000 ng/mL. The lower limit of quantification was 25 ng/mL. The intra- and inter-day precision(relative standard deviation) and accuracy(relative error) values were within 12.4%. Each plasma sample was analyzed within 3 min.展开更多
采用微波辅助提取法,以50%乙醇作为提取剂,提取野菜鼠曲草中的黄酮类化合物,提取物经AB-8大孔树脂纯化后,利用高效液相色谱电喷雾离子化串联质谱(high performance liquid chromatography electrospray ionization tandem mass spectrom...采用微波辅助提取法,以50%乙醇作为提取剂,提取野菜鼠曲草中的黄酮类化合物,提取物经AB-8大孔树脂纯化后,利用高效液相色谱电喷雾离子化串联质谱(high performance liquid chromatography electrospray ionization tandem mass spectrometry,LC-ESI-MS/MS)结合标准品比对法对其组成进行分析,从中鉴定出8种黄酮和3种酚酸类化合物:3,5-二咖啡酰奎宁酸(4.957μg/mg)、绿原酸(2.144μg/mg)、奎宁酸(1.073μg/mg)、毛地黄黄酮(0.884μg/mg)、紫云英苷(0.777μg/mg)、金丝桃苷(0.486μg/mg)、芹菜素-7-葡萄糖苷(0.327μg/mg)、槲皮素-3-O-槐糖苷(0.144μg/mg)、槲皮素(0.072μg/mg)、木犀草苷(0.066μg/mg)和野黄芩苷(0.056μg/mg)。其中奎宁酸、芹菜素-7-葡萄糖苷、紫云英苷、槲皮素-3-O-槐糖苷在该植物中尚属首次发现。展开更多
A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry(LC-ESI-MS/MS)method was established to simultaneously quantitate four categories of compounds(isoflavonoids,flavonoids,al...A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry(LC-ESI-MS/MS)method was established to simultaneously quantitate four categories of compounds(isoflavonoids,flavonoids,alkaloids and saponins)in Gegen-Qinlian decoction(GQD).These compounds were separated by a Shiseido CAPCELL PAK C18 column with a linear gradient consisting of 0.1%(v/v)formic acid in water(A)and 0.1%(v/v)formic acid in acetonitrile(B),and delivered at a flow rate of 0.3 mL/min.All the analytes were determined by electrospray positive ionization tandem mass spectrometry in a multiple reaction monitoring(MRM)mode.Linearity,accuracy,precision,recovery and stability of the method were evaluated with the validation over the range of 4.0-538 5 ng/mL.The proposed method was applied to the analysis of a Chinese herbal preparation GQD successfully.展开更多
文摘The ginkgo terpenoids including bilobalide and ginkgolides are the main pharmaceutical components in the leaves or extracts of Ginkgo biloba L. In this paper, the analysis of bilobalide and ginkgolides in leaves of Ginkgo biloba L. by high performance liquid chromatography (HPLC)-electrospray ionization (ESI)-mass spectrometry (MS) was carried out. The separation was performed on Inertsil ODS3 column with methanol-water (36:64) as mobile phase, with 1 mL·min -1 of flow rate at 35℃. Then the mass spectrum analysis was conducted by ZMD micromass electrospray ionization (ESI)-mass spectrometer (MS). The HPLC total ion chromatogram and selected ion chromatogram (with 325, 407, 423, 439 of m/z) of the sample and ESI-/MS mass spectra of the peaks in the chromatograms were obtained. So bilobalide, ginkgolide A, B, C and J in Ginkgo biloba L. leaves were identified. The method is easy and rapid, with a good accuracy.
文摘A sensitive and selective liquid chromatography-electrospray ionization tandem mass spectrometry（LC- ES1-MS/MS） was used for the simultaneous determination of metformin and glimepiride in beagle dog plasma with glipizide as internal standard（IS）. After simplified protein precipitation with methanol, both the analytes and IS were chromatographed on a Zorbax CN column via gradient elution with methanol（containing 5 mmol/L ammonium ace- tate） and 5 mmol/L aqueous ammonium acetate as the mobile phase. Detection was performed by multiple reaction monitoring（MRM） scanning via ESI source operated in positive ionization mode. Specificity, linearity, accuracy, pre- cision, recovery, matrix effect and stability were validated for metformin and glimepiride in beagle dog plasma. The calibration curves were linear in a concentration range of 10-10000 ng/mL for metformin and 4-4000 ng/mL for glimepiride with both correlation coefficients higher than 0.99. The recoveries obtained for the analytes and IS were all between 82.7% and 101.2%. The method exhibited excellent performance in terms of selectivity, robustness, short analytical time and simplicity of sample preparation. Finally, the proposed method was applied to a bioequivalence study of self-made bilayer tablet and commercial formulation containing 500 mg of metformin and 1 mg of glimepi- ride in beagle dogs.
文摘In this paper, a sensitive and specific liquid chromatography-electrospray ionisation-mass spectrometry （LC-ESI-MS） method has been developed and validated for the identification and determination of seven flavonoids, namely epimedin A, epimedin B, epimedin C, icariin, sagittatoside B, 2＂-O-rhamnosyl icariside II, and baohuoside I in Epimedium from different sources.
基金support provided by the National Natural Science Foundation of China(Grant No.:82173776)Natural Science Foundation of Guangdong Province,China(Grant No.:2021A1515010574)Guangdong Basic and Applied Basic Research Foundation,China(Grant No.:2021A1515110346).
文摘Liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS)is a widely utilized technique for in vivo pharmaceutical analysis.Ionization interference within electrospray ion source,occurring between drugs and metabolites,can lead to signal variations,potentially compromising quantitative accuracy.Currently,method validation often overlooks this type of signal interference,which may result in systematic errors in quantitative results without matrix-matched calibration.In this study,we conducted an investigation using ten different groups of drugs and their corresponding metabolites across three LC-ESI-MS systems to assess the prevalence of signal interference.Such interferences can potentially cause or enhance nonlinearity in the calibration curves of drugs and metabolites,thereby altering the relationship between analyte response and concentration for quantification.Finally,we established an evaluation scheme through a step-by-step dilution assay and employed three resolution methods:chromatographic separation,dilution,and stable labeled isotope internal standards correction.The above strategies were integrated into the method establishment process to improve quantitative accuracy.
文摘A rapid and sensitive liquid chromatography tandem mass spectrometry(LC-MS/MS) method has been developed and validated for the determination of moxifloxacin(MOXI) in human plasma. After a simple protein precipitation using acetonitrile, the post treatment samples were analysed on a C18 column interfaced with a Triple Quadropole Tandem Mass Spectrometer. Positive electrospray ionization was employed as the ionization source. The mobile phase consisted of 0.1% formic acid–acetonitrile(60:40, v/v). Ciprofloxacin(CIPRO) was used as an internal standard. The analyte and internal standard(CIPRO) were monitored in the multiple reaction monitoring mode(MRM). The mass transition ion-pair has been followed as m/z 402→358.2 for MOXI and 332→288.1 for CIPRO. The method was linear in the concentration range of 25–5000 ng/mL. The lower limit of quantification was 25 ng/mL. The intra- and inter-day precision(relative standard deviation) and accuracy(relative error) values were within 12.4%. Each plasma sample was analyzed within 3 min.
文摘采用微波辅助提取法,以50%乙醇作为提取剂,提取野菜鼠曲草中的黄酮类化合物,提取物经AB-8大孔树脂纯化后,利用高效液相色谱电喷雾离子化串联质谱(high performance liquid chromatography electrospray ionization tandem mass spectrometry,LC-ESI-MS/MS)结合标准品比对法对其组成进行分析,从中鉴定出8种黄酮和3种酚酸类化合物:3,5-二咖啡酰奎宁酸(4.957μg/mg)、绿原酸(2.144μg/mg)、奎宁酸(1.073μg/mg)、毛地黄黄酮(0.884μg/mg)、紫云英苷(0.777μg/mg)、金丝桃苷(0.486μg/mg)、芹菜素-7-葡萄糖苷(0.327μg/mg)、槲皮素-3-O-槐糖苷(0.144μg/mg)、槲皮素(0.072μg/mg)、木犀草苷(0.066μg/mg)和野黄芩苷(0.056μg/mg)。其中奎宁酸、芹菜素-7-葡萄糖苷、紫云英苷、槲皮素-3-O-槐糖苷在该植物中尚属首次发现。
基金supported by the National Natural Science Foundation of China(No.90202039)"Chen Guang" Project for Personnel Cultivation of Shanghai Municipal Education Commission(No.09CG43)the Construction Program for Innovative Research Teamin Shanghai Institutions of Higher Education
文摘A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry(LC-ESI-MS/MS)method was established to simultaneously quantitate four categories of compounds(isoflavonoids,flavonoids,alkaloids and saponins)in Gegen-Qinlian decoction(GQD).These compounds were separated by a Shiseido CAPCELL PAK C18 column with a linear gradient consisting of 0.1%(v/v)formic acid in water(A)and 0.1%(v/v)formic acid in acetonitrile(B),and delivered at a flow rate of 0.3 mL/min.All the analytes were determined by electrospray positive ionization tandem mass spectrometry in a multiple reaction monitoring(MRM)mode.Linearity,accuracy,precision,recovery and stability of the method were evaluated with the validation over the range of 4.0-538 5 ng/mL.The proposed method was applied to the analysis of a Chinese herbal preparation GQD successfully.
