Journal
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
Volume 78-79, Issue -, Pages 123-128Publisher
ELSEVIER
DOI: 10.1016/j.jpba.2013.02.006
Keywords
Indomethacin; LC-MS; Plasma; Urine; Method validation
Categories
Funding
- Eunice Kennedy Shriver National Institute of Child Health and Human Development (NICHD), Obstetric Pharmacology Research Unit Network (OPRU) G.D.V. Hankins [U10HD047891]
- National Institute of Allergy and Infectious Diseases (NIAID), the NICHD, and the Office of the Director (OD), National Institutes of Health [K12HD052023]
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A liquid chromatography with single quadrupole mass spectrometry method was developed for the quantitative determination of indomethacin in the maternal plasma and urine of pregnant patients under treatment. A deuterium-labeled isotope of indomethacin (d(4)-indomethacin) was used as an internal standard. The maternal plasma and urine samples were acidified with 1.0 M HCl then extracted with chloroform to achieve the extraction recovery range of 94-104% with variation less than 11%. Chromatographic separation was achieved by a Waters Symmetry C-18 column with isocratic elution of 0.05% (v/v) formic acid aqueous solution and acetonitrile (47:53, v/v). An in-source fragmentation was applied on the single quadrupole mass spectrometer equipped with an electrospray ionization source at positive mode. The LC-ESI-MS quantification was performed in the selected ion monitoring mode targeting ions at m/z 139 for indomethacin and m/z 143 for its internal standard. The calibration curves were linear in the concentration ranges between 14.8 and 2.97 x 10(3) ng/mL for plasma samples and between 10.5 and 4.21 x 10(3) ng/mL for urine samples. The relative standard deviation of this method was less than 8% for intra- and inter-day assays, and the accuracy ranged between 90% and 108%. (C) 2013 Elsevier B.V. All rights reserved.
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