Determination of pregabalin in human plasma by electrospray ionisation tandem mass spectroscopy

The present study was undertaken to develop a validated, rapid, simple, and low-cost ultraviolet (UV) spectrophotometric method for estimating Etoricoxib (ETX) in pharmaceutical formulations. The analysis was performed on λ max 233 nm using 0.1 M HCl as blank/diluent. The proposed method was validated on International Conference on Harmonization (ICH) guidelines including parameters as linearity, accuracy, precision, reproducibility, and specificity. The proposed method was also used to access the content of the ETX in two commercial brands of Indian market. Beer's law was obeyed in concentration range of 0.1–0.5 μg/ml, and the regression equation was Y = 0.418x + 0.018. The mean accuracy values for 0.1 μg/ml and 0.2 μg/ml concentration of ETX were found to be 99.76 ± 0.52% and 99.12 ± 0.84, respectively, and relative standard deviation (RSD) of interday and intraday was less than 2%. The developed method was suitable and specific to the analysis of ETX even in the presence of common excipients. The method was applied on two different marketed brands and ETX contents were 98.5 ± 0.56 and 99.33 ± 0.44, respectively, of labeled claim. The proposed method was validated as per ICH guidelines and statistically good results were obtained. This method can be employed for routine analysis of ETX in bulk and commercial formulations.

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“…at room temperature and at 18°C. [14] The respective absorbance of 0.3 μg/ml was noted and the result was indicated as %RSD [Table 3]. …”

Section: Resultsmentioning

confidence: 99%

A simple Ultraviolet spectrophotometric method for the determination of etoricoxib in dosage formulations

Singh¹,

Mishra²,

Verma³

et al. 2012

J Adv Pharm Technol Res

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“…3 Therefore, its determination in biological fluids, by a simple and sensitive analytical method, can help in dose adjustments and toxicity prevention. Different analytical methods have been employed for determination of pregabalin in a variety of matrices such as spectrophotometry, 4,5 spectrofluorimetry, 6 gas chromatography, 7 high-performance liquid chromatographymass spectrometry (HPLC-MS), [8][9][10] ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), [11][12][13] electrospray ionisation-tandem mass spectrometry (ESI-MS/MS), 14 and nuclear magnetic resonance spectroscopy (NMR). 15 However, only a few studies were performed based on capillary electrophoresis (CE) separation for quantification of pregabalin.…”

Section: Introductionmentioning

confidence: 99%

Development of a Micellar Electrokinetic Chromatographic Method with Indirect UV Detection for Pregabalin Determination in Serum Samples

et al. 2018

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Background: A micellar electrokinetic chromatographic (MEKC)/ indirect UV detection method with hydrodynamic and electrokinetic injection has been developed for the determination of pregabalin in the serum samples. Methods: Separation of the drug was achieved on Agilent capillary electrophorese in less than 5 min using a 50 cm × 75 μm i.d. uncoated fused-silica capillary and a background electrolyte (BGE) consisting of 5-aminosalicylic acid (5-ASA, 10 mmol L-1), cetyl trimethylammonium bromide (CTAB, 1 mmol L-1) and tri-sodium citrate (4% w/v). The influence of various parameters on the separation such as separation voltage, injection time, cassette temperature, pH of BGE and organic modifier was investigated. Results: Method validation shown good linearity (R2> 0.999) in the range of 1.5-100 µg mL-1 of pregabalin. A limit of detection (LOD) of 0.8 μg mL-1 and a limit of quantitation (LOQ) of 2.6 μg mL-1 were reported for pregabalin. Conclusion: The proposed method was found to be suitable and accurate for the determination of pregabalin in serum samples.

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“…For determination of pregabalin in biological fluids, sophisticated methods such as methods based on LC-MS-MS were employed [11][12][13][14]. Although most of LC-MS-MS methods are sensitive and reliable, the instruments are too expensive and unavailable in most of clinical laboratories.…”

Section: Introductionmentioning

confidence: 99%

Validated HPLC Method for Quantification of Pregabalin in Human Plasma Using 1-Fluoro-2,4-dinitrobenzene as Derivatization Agent

Ahmadkhaniha

Mottaghi

Zargarpoor

et al. 2014

Chromatography Research International

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In this study, a sensitive, simple, and reliable HPLC method for quantification of pregabalin in human plasma was developed and validated. 1-Fluoro-2,4-dinitrobenzene was used as precolumn derivatization agent. For chromatography, an analytical reversed phase (C18) column and a mixture of Na2HPO410 mM (pH 8.0)—methanol (35 : 65 v/v) were used as stationary and mobile phase, respectively. Detection was performed using a UV detector tuned at 360 nm. The linearity of the method was tested over the concentration range 1–4500 ng/mL in 500 μL of human plasma and satisfactory results were obtained (r2> 0.999). The method showed good precision and accuracy in terms of within—between days relative standard deviations and percent deviation from nominated values (in the range of 4.3–12.7% and 2.6–8.0%, resp.). The limit of quantification of the method was found to be 1 ng/mL which is better than previously reported method and indicates its potential application for sensitive bioanalysis.

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Determination of pregabalin in human plasma by electrospray ionisation tandem mass spectroscopy

Cited by 35 publications

References 9 publications

A simple Ultraviolet spectrophotometric method for the determination of etoricoxib in dosage formulations

A simple Ultraviolet spectrophotometric method for the determination of etoricoxib in dosage formulations

Development of a Micellar Electrokinetic Chromatographic Method with Indirect UV Detection for Pregabalin Determination in Serum Samples

Validated HPLC Method for Quantification of Pregabalin in Human Plasma Using 1-Fluoro-2,4-dinitrobenzene as Derivatization Agent

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