A sensitive UPLC-APCI-MS/MS method for the determination of dexamethasone and its application in an ocular tissue distribution study in rabbits following topical administration

A sensitive, specific and rapid ultra-performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (UPLC-APCI-MS/MS) method has been developed and validated for the determination of dexamethasone (DEX) in ocular tissues and biofluids of rabbits. Dexamethasone-d...

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Bibliographic Details
Published in:Analytical methods 2018-01, Vol.1 (2), p.237-2316
Main Authors: Matta, Murali K, Narayanasamy, Suresh, Thomas, Christopher D, Xu, Lin, Stewart, Sharron, Chockalingam, Ashok, Patel, Vikram, Rouse, Rodney
Format: Article
Language:English
Subjects:
Ammonium
Bovine serum albumin
Buffers
Calibration
Chromatography
Dexamethasone
Flow velocity
Formic acid
Ionization
Ions
Liquid chromatography
Mass spectrometry
Mass spectroscopy
Precipitation
Proteins
Rabbits
Rainfall
Serum albumin
Tobramycin
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Summary:A sensitive, specific and rapid ultra-performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (UPLC-APCI-MS/MS) method has been developed and validated for the determination of dexamethasone (DEX) in ocular tissues and biofluids of rabbits. Dexamethasone-d 5 (DEX-d 5 ) was used as an internal standard. Protein precipitation was used to extract the drug from ocular tissue homogenates, biofluids and plasma. Chromatographic separation was achieved on an Acquity C 18 column (100 × 2.1 mm, 1.7 μm) using a gradient run with a mobile phase composed of methanol and 5 mM ammonium formate in 0.1% formic acid in water buffer at a flow rate of 0.5 mL min −1 . A detailed method validation in two matrices (bovine serum albumin and phosphate buffer) was performed as per the FDA guidelines and the calibration curve obtained was linear ( r 2 = 999) over the concentration range 200-100 000 pg mL −1 . A Sciex 6500+ coupled with a Waters Acquity UPLC (Ultra Performance Liquid Chromatography) system was operated in the multiple monitoring mode (MRM) during the analysis. The proposed method was applied to a rabbit ocular tissue distribution study after topical ophthalmic administration of dexamethasone and tobramycin suspension. A sensitive, specific and rapid ultra-performance liquid chromatography tandem mass spectrometry method has been developed and validated for the determination of dexamethasone (DEX) in ocular tissues of rabbits.
ISSN:1759-9660
1759-9679
DOI:10.1039/c8ay00283e