Science and Technology Production
Article
Authorship
Boscolo, Oriana
;
FLOR, SABRINA ANDREA
;
Dobrecky Ceciclia
;
MARTINEFSKI, MANUELA ROMINA
;
TRIPODI, VALERIA PAULA
;
LUCANGIOLI, SILVIA EDITH
Date
2018
Publishing House and Editing Place
DAVID PUBLISHING
Magazine
Journal of Pharmacy and Pharmacology,
vol. 5
(pp. 448-455)
- ISSN 2328-2150
DAVID PUBLISHING
DAVID PUBLISHING
ISSN
2328-2150
Summary
Information provided by the agent in
SIGEVA
Abstract: Objective: To develop a highly sensitive LC-MS/MS (liquid chromatography-mass spectrometry/mass spectrometry)method applied to the detection and quantitation of UDCA (ursodeoxycholic acid) related substances such as CA (cholic acid), DCA(deoxycholic acid), CDCA (chenodeoxycholic acid) and LCA (lithocholic acid) in raw material and pharmaceutical formulation.Methods: The method was validated for specificity, linearity, accuracy, precision, robustness. A triple quadrupole mass detector ...
Abstract: Objective: To develop a highly sensitive LC-MS/MS (liquid chromatography-mass spectrometry/mass spectrometry)method applied to the detection and quantitation of UDCA (ursodeoxycholic acid) related substances such as CA (cholic acid), DCA(deoxycholic acid), CDCA (chenodeoxycholic acid) and LCA (lithocholic acid) in raw material and pharmaceutical formulation.Methods: The method was validated for specificity, linearity, accuracy, precision, robustness. A triple quadrupole mass detector wasemployed, equipped with an ESI (electrospray ionization) source operated in the negative ion mode. The chromatographic systemconsisted of a Symmetry C18 column (150 mm × 4.6 mm, id; particle size 5 µm) and methanol-acetonitrile-ammonium acetate (pH 7.6;10 mM) (40:40:20, v/v/v) as the mobile phase. The chromatographic conditions were 25 uL injection volume, flow rate of 0.4 mL/minand column temperature set at 35 °C. Key findings: The method requires a minimum sample amount and presents very low LOD(limits of detection) for CA (0.29 ng/mL), DCA (0.59 ng/mL), CDCA (0.13 ng/mL) and LCA (0.44 ng/mL) in comparison to LCmethods coupled to different detectors like UV (ultraviolet), fluorescence and refractive index. Conclusions: The developed andvalidated LC-MS/MS method for the determination of UDCA and related substances in raw material and in a suspension wasadvantageous since it required a minimum sample amount. In turn, it could be used as a stability indicating method.
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Key Words
RAW MATERIALPHARMACEUTICAL FORMULATIONURSODEOXYCHOLIC ACIDLC-MS/MSRELATED SUBSTANCES
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