Liquid Chromatography/Tandem Mass Spectrometry for the Simultaneous Determination of Ursodiol and its Major Metabolites, Tauroursodeoxycholic Acid and Glycoursodeoxycholic Acid in Human Plasma
A rapid and sensitive method is described for the quantification of ursodiol and its major metabolites glycoursodeoxycholic acid (GUDCA) and tauroursodeoxycholic acid (TUDCA) in human plasma using single internal standard (Ursodeoxycholic Acid d4). Solid phase extraction was performed and chromatogr...
Saved in:
| Main Authors: | , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
Wiley
2012-01-01
|
| Series: | E-Journal of Chemistry |
| Online Access: | http://dx.doi.org/10.1155/2012/181672 |
| Tags: |
Add Tag
No Tags, Be the first to tag this record!
|
| _version_ | 1832563527431225344 |
|---|---|
| author | M. Ganesan S. Nanjundan S. Viswanathan G. Uma |
| author_facet | M. Ganesan S. Nanjundan S. Viswanathan G. Uma |
| author_sort | M. Ganesan |
| collection | DOAJ |
| description | A rapid and sensitive method is described for the quantification of ursodiol and its major metabolites glycoursodeoxycholic acid (GUDCA) and tauroursodeoxycholic acid (TUDCA) in human plasma using single internal standard (Ursodeoxycholic Acid d4). Solid phase extraction was performed and chromatographic separation of 5µL injected sample was achieved using Waters Xterra, 5µm column with a mobile phase comprised of methanol and 5 mM ammonium formate with 0.1 % acetic acid ( 70 : 30, v/v ). The mass spectrometer was used in negative ion mode and multiple reactions monitoring using electro spray ionization mode as an interface. The method was fully validated and the calibration curves were linear over the concentration range of 25.9 to 15300.1 ng/mL for ursodiol, 2.7 to 1587.5ng/mLfor tauroursodeoxycholicacid and 25.4 to 15040.9 ng/mL for glycoursodeoxycholic acid. The method was sensitive and specific, with the lower limit of quantification of 25.9, 2.7 and 25.4 ng/ml for ursodiol, tauroursodeoxycholic acid and glycoursodeoxycholic acid respectively. The present method includes a simple and rapid sample preparation with shorter analysis run time and less flow rate compared to previously reported methods. The method was applied successfully for a bioequivalence study in healthy subjects. |
| format | Article |
| id | doaj-art-e0b0147c56344de584236633c1dad592 |
| institution | Kabale University |
| issn | 0973-4945 2090-9810 |
| language | English |
| publishDate | 2012-01-01 |
| publisher | Wiley |
| record_format | Article |
| series | E-Journal of Chemistry |
| spelling | doaj-art-e0b0147c56344de584236633c1dad5922025-02-03T01:20:05ZengWileyE-Journal of Chemistry0973-49452090-98102012-01-01931605161210.1155/2012/181672Liquid Chromatography/Tandem Mass Spectrometry for the Simultaneous Determination of Ursodiol and its Major Metabolites, Tauroursodeoxycholic Acid and Glycoursodeoxycholic Acid in Human PlasmaM. Ganesan0S. Nanjundan1S. Viswanathan2G. Uma3Department of Chemistry, Anna University, Chennai-600025, IndiaDepartment of Chemistry, Anna University, Chennai-600025, IndiaMicro Therapeutic Research Labs Private Limited, Chennai-600 059, IndiaC. LBaid Metha College of Pharmacy, Chennai-600 097, IndiaA rapid and sensitive method is described for the quantification of ursodiol and its major metabolites glycoursodeoxycholic acid (GUDCA) and tauroursodeoxycholic acid (TUDCA) in human plasma using single internal standard (Ursodeoxycholic Acid d4). Solid phase extraction was performed and chromatographic separation of 5µL injected sample was achieved using Waters Xterra, 5µm column with a mobile phase comprised of methanol and 5 mM ammonium formate with 0.1 % acetic acid ( 70 : 30, v/v ). The mass spectrometer was used in negative ion mode and multiple reactions monitoring using electro spray ionization mode as an interface. The method was fully validated and the calibration curves were linear over the concentration range of 25.9 to 15300.1 ng/mL for ursodiol, 2.7 to 1587.5ng/mLfor tauroursodeoxycholicacid and 25.4 to 15040.9 ng/mL for glycoursodeoxycholic acid. The method was sensitive and specific, with the lower limit of quantification of 25.9, 2.7 and 25.4 ng/ml for ursodiol, tauroursodeoxycholic acid and glycoursodeoxycholic acid respectively. The present method includes a simple and rapid sample preparation with shorter analysis run time and less flow rate compared to previously reported methods. The method was applied successfully for a bioequivalence study in healthy subjects.http://dx.doi.org/10.1155/2012/181672 |
| spellingShingle | M. Ganesan S. Nanjundan S. Viswanathan G. Uma Liquid Chromatography/Tandem Mass Spectrometry for the Simultaneous Determination of Ursodiol and its Major Metabolites, Tauroursodeoxycholic Acid and Glycoursodeoxycholic Acid in Human Plasma E-Journal of Chemistry |
| title | Liquid Chromatography/Tandem Mass Spectrometry for the Simultaneous Determination of Ursodiol and its Major Metabolites, Tauroursodeoxycholic Acid and Glycoursodeoxycholic Acid in Human Plasma |
| title_full | Liquid Chromatography/Tandem Mass Spectrometry for the Simultaneous Determination of Ursodiol and its Major Metabolites, Tauroursodeoxycholic Acid and Glycoursodeoxycholic Acid in Human Plasma |
| title_fullStr | Liquid Chromatography/Tandem Mass Spectrometry for the Simultaneous Determination of Ursodiol and its Major Metabolites, Tauroursodeoxycholic Acid and Glycoursodeoxycholic Acid in Human Plasma |
| title_full_unstemmed | Liquid Chromatography/Tandem Mass Spectrometry for the Simultaneous Determination of Ursodiol and its Major Metabolites, Tauroursodeoxycholic Acid and Glycoursodeoxycholic Acid in Human Plasma |
| title_short | Liquid Chromatography/Tandem Mass Spectrometry for the Simultaneous Determination of Ursodiol and its Major Metabolites, Tauroursodeoxycholic Acid and Glycoursodeoxycholic Acid in Human Plasma |
| title_sort | liquid chromatography tandem mass spectrometry for the simultaneous determination of ursodiol and its major metabolites tauroursodeoxycholic acid and glycoursodeoxycholic acid in human plasma |
| url | http://dx.doi.org/10.1155/2012/181672 |
| work_keys_str_mv | AT mganesan liquidchromatographytandemmassspectrometryforthesimultaneousdeterminationofursodiolanditsmajormetabolitestauroursodeoxycholicacidandglycoursodeoxycholicacidinhumanplasma AT snanjundan liquidchromatographytandemmassspectrometryforthesimultaneousdeterminationofursodiolanditsmajormetabolitestauroursodeoxycholicacidandglycoursodeoxycholicacidinhumanplasma AT sviswanathan liquidchromatographytandemmassspectrometryforthesimultaneousdeterminationofursodiolanditsmajormetabolitestauroursodeoxycholicacidandglycoursodeoxycholicacidinhumanplasma AT guma liquidchromatographytandemmassspectrometryforthesimultaneousdeterminationofursodiolanditsmajormetabolitestauroursodeoxycholicacidandglycoursodeoxycholicacidinhumanplasma |