Sensitive and selective liquid chromatography–tandem mass spectrometry method for the determination of metoclopramide in human plasma: application to a bioequivalence study

Abstract

A simple, sensitive and rapid method has been developed and validated for determination of the metoclopramide (MCP) in 100 microL human plasma. The analytical procedure involves a liquid-liquid extraction method using tramadol as an internal standard (IS). Chromatographic separation was carried out on a HyPURITY ADVANCE column using a mobile phase consisting of acetonitrile and 10 mm ammonium acetate buffer in the ratio of 80:20 (v/v) at a flow rate of 0.3 mL/min. The total run time of analysis was 2.5 min and elution of MCP and IS occurred at 0.9 and 1.3 min, respectively. A linear response function was established for the range of concentrations 0.53-42.07 ng/mL (r > 0.99). The intra- and inter-day precision values for MCP met the acceptance as per FDA guidelines. MCP was stable in a battery of stability studies viz., bench-top, auto-sampler and freeze-thaw cycles. The developed assay method was successfully applied to an oral bioequivalence study in humans.

Simultaneous quantification of niacin and its three main metabolites in human plasma by LC–MS/MS

“…Hence NA and its metabolites display complexities in their physico-chemical properties that may have to be carefully addressed during the sample clean-up process for an optimal/efficient recovery of all the analytes. For the plasma samples clean-up process, various extraction techniques, PPT, LLE and SPE have been reported [18][19][20][21][22][23]27]. In the present study, the LLE was not feasible due to the low extraction recovery.…”

“…However, the main metabolite NUA was not quantified and the method was only applied to rat plasma [22]. Hitherto to the best of our knowledge there was one LC-MS/MS method reported for the simultaneous quantification of NA, NAM, NUA and 2-Pyr in human plasma [21], the samples were prepared with LLE, which has been reported not applicable to NA [18,23]. Moreover, endogenous NAM and 2-Pyr were not found in human blank plasma in that article.…”

“…Previous publications have described several methods for determination of NA or NA along with its metabolites in plasma [8][9][10][11][12][13][14][15][16][17][18][19][20][21][22], including many HPLC-UV/FD methods [8][9][10][11][12][13][14][15][16][17] and a few LC-MS/MS methods [18][19][20][21][22]. Pfuhl et al [20] have discussed the drawbacks of the various methods reported and established an LC-MS/MS method.…”

Potentiometric Sensors Based on MF-4SC Membranes and Carbon Nanotubes for the Determination of Nicotinic Acid in Aqueous Solutions and Pharmaceuticals

“…The necessity to analyze objects with a complex composition gives an impetus to the development of new methods for the determination of nicotinic acid [1][2][3][4][5][6][7][8][9][10][11]. Several reports focus on the use of mass spectrometry [1,2], high-performance liquid chromatography combined with mass spectrometry [3,4], voltammetry [4][5][6], and solid phase extraction [7] for this purpose. There are reports on methods for determining trace amounts of nicotinic acid in physiological fluids that are based on acid sorption on modified carbon dots and subsequent fluorometric detection [8] and methods using voltammetric [9] and amperometric [10] sensors.…”

Resolution and quantification challenge of modern chemometric models in the determination of anti-migraine tablets containing ergotamine, caffeine, acetaminophen, and metoclopramide

“…It acts as a stimulant of the central nervous system (CNS) and is sometimes given with ERG in formulations for the treatment of migraine. 6 Several analytical procedures have been described for the simultaneous determination of mixtures containing PAR and CAF, including spectrophotometry, 7 chemometrics, 8 highperformance thin-layer chromatography (HPTLC), 9 highperformance liquid chromatography (HPLC), [10][11][12] and gas chromatography. 13 The United States Pharmacopeia (USP) 14 describes the determination of ERG and CAF tablets by HPLC with uorimetric detection for ERG at l em ¼ 435 nm and l ex ¼ 325 nm, and ultraviolet (UV) detection for CAF at 254 nm.…”