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Banda J.,QPS Bioserve India Pvt. Ltd | Lakshmanan R.,QPS Bioserve India Pvt. Ltd | Vvs S.P.,QPS Bioserve India Pvt. Ltd | Gudla S.P.,QPS Bioserve India Pvt. Ltd | Prudhivi R.,QPS Bioserve India Pvt. Ltd
Biomedical chromatography : BMC | Year: 2015

A simple and high sensitive ultra-high-performance liquid chromatography tandem mass spectrometry method for the determination of fludrocortisone in human plasma was developed and validated as per guidelines. The analyte and internal standard (IS), fludrocortisone-d5 , were extracted from human plasma via liquid-liquid extraction using tert-butyl methyl ether. The chromatographic separation was achieved on a Chromolith RP18e column using a mixture of acetonitrile and 2 mm ammonium formate (70:30, v/v) as the mobile phase at a flow rate of 0.7 mL/min. Quantitation was performed on a triple quadrupole mass spectrometer employing electrospray ionization technique, operating in multiple reaction monitoring and positive ion mode. The precursors to product ion transitions monitored for fludrocortisone and IS were m/z 381.2 → 343.2 and 386.2 → 348.4, respectively. The assay was validated with linear range of 40-3000 pg/mL. The intra- and inter-day precisions (relative standard deviation) were within 0.49-7.13 and 0.83-5.87%, respectively. The proposed method was successfully applied to pharmacokinetic studies in humans. Copyright © 2015 John Wiley & Sons, Ltd.

Banda J.,QPS Bioserve India Pvt. Ltd | Lakshmanan R.,QPS Bioserve India Pvt. Ltd | Katepalli R.B.,QPS Bioserve India Pvt. Ltd | Reddy Venati U.K.,QPS Bioserve India Pvt. Ltd | And 2 more authors.
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences | Year: 2016

Olsalazine sodium, salicylate derivative (prodrug) is effectively bioconverted to mesalazine (5-aminosalicylic acid; 5-ASA), which has an anti-inflammatory activity in ulcerative colitis. In this article, a novel highly sensitive and selective method was developed and validated to determine mesalazine in human plasma using a derivatization technique to enhance the signal intensity by using ultra- high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) with an electrospray ionization interface. The sample preparation consisted of a derivatization with propionyl anhydride followed by liquid liquid extraction (LLE) to remove the interference and minimize the matrix effect of human plasma. The multiple reaction monitoring (MRM) mode of the negative ion was performed and the transitions of m/z 208.1 → 107.0 and m/z 211.1 → 110.1 were used to measure the derivative of mesalazine and mesalazine-d3. The chromatographic separation was achieved using kinetex XB-C18 (100 × 4.6 mm 2.6 μ) analytical column with 0.1% formic acid in water and acetonitrile as mobile phase with a gradient elution. Nominal retention times of mesalazine and IS were 3.08 and 3.07 min, respectively. Absolute recovery was found to be between 82-95% for analyte and about 78% for IS. The standard curves was linear (r2 > 0.995) in the concentration range 0.10 to 12.0 ng/mL with lower limit of quantification (LLOQ) in human plasma was 0.10ng/mL. The average intra-day/inter-day precision values (%CV) were in the range from 0.6-2.9 % and 1.3-3.8 %, respectively, while the average accuracy value was 103.8-107.2%. This method has been successfully applied to the human pharmacokinetics of olsalazine sodium 250mg capsules following single oral administration. © 2015 Elsevier B.V.

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