Development and Validation of a LC Method for the Determination of Pramipexole Using an Experimental Design

Gedela, Srinubabu; Jaganbabu, K.; Sudharani, B.; Venugopal, K R; Girizasankar, G.; Rao, J. V. L. N. Seshagiri

doi:10.1365/s10337-006-0829-3

Cited by 35 publications

(20 citation statements)

References 13 publications

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“…The eventual objective of RSM is to determine the optimum operating conditions for the system or to determine a region of the factor space in which operating requirements are satisfied. As demonstrated by Srinubabu et al during the validation of robustness and intermediate precision for voriconazole 15) and pramipexole 16) in pharmaceutical dosage forms using response surface methodology, the use of experimental design during optimization made the validation process easier and more cost effective.…”

Section: Development and Validation Of Lc-ms/ms Methods For The Quantimentioning

confidence: 99%

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Development and Validation of LC-MS/MS Method for the Quantification of Oxcarbazepine in Human Plasma Using an Experimental Design

Gedela

Ratnam

Rao

et al. 2008

CHEMICAL & PHARMACEUTICAL BULLETIN

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Oxcarbazepine (OXB) is a newer antiepileptic drug indicated for the treatment of partial seizures as both monotherapy and combination therapy in adults and children with epilepsy. At present, determinations of OXB have been established by the use of HPLC-UV spectrometry, [1][2][3] or LC-APCI-MS mass-spectrometry. 4) However, none of these methods achieved the quick quantification and identification of OXB in a single run. Although methods for simultaneous determination of OXB and some of antiepileptic drugs has been described, 5-11) they were not particular interest since it takes too long chromatographic run time especially when applied to OXB, and had low sensitivity; it appeared that no assay existed for determination of the OXB using HPLC-MS/MS. The assay described here requires small mobile phase and sample volume, short chromatographic run and is sensitive, specific and fully validated.Optimization of an MS response includes methods to improve the abundance of a specific precursor or product ion, or yielding as comprehensive or selective measurements as possible (Table 1). Maximization of the signal or the signal-tonoise ratio (S/N) of a particular ion can be used for quantitative optimization, but choosing qualitative optimization criteria are less trivial.Optimization techniques of particular interest are factorial design and central composite design, for screening of the important parameters Placket-Burman design can be useful. Chemometric approaches for optimization of ESI or MS/MS parameters also occur in literature. 12,13) In this present study Plackett-Burman and factorial designs are employed for screening of essential parameters and optimization respectively. ExperimentalChemicals and Reagents OXB, and imipramine (Internal standard), were kindly provided by Glenmark Pharmaceuticals (Mumbai, India). HPLC-grade acetonitrile, methanol, formic acid and diethyl ether were purchased from Qualigens (Mumbai, India). Blank human plasma was harvested after 5 min centrifugation at 4000ϫg and stored at Ϫ20°C until use.Instrumentation The HPLC system consisted of an HP1100 binary pump, auto sampler, column oven, and online degasser (Agilent Technologies, Palo Alto, CA, U.S.A.). The analytical column used was reversedphase symmetry C18 (75 mmϫ4.6 mm i.d. 3.5 mm). A mobile phase of 10 mM ammonium formate/ACN (10 : 90, v/v) was pumped at a flow rate of 0.3 ml/min and the injected sample volume to whole over the method is 10 ml. The LC elute was introduced directly into an Applied Biosystems triple quadrupole mass spectrometer API 4000 (MDS-Sciex, Toronto Canada, software: Analyst 1.4.1) equipped with an electrospray ionization source. The triple quadrupole mass spectrometer was operated in the positive ion mode and the multiple reaction monitoring (MRM) chromatograms obtained were used for quantification. MRM transitions of m/z 253→208, m/z and 281→86 were respectively optimized for OXB and Imipramine. The 28Vol. 56, No. 1 A rapid tandem mass spectrometric (MS-MS) method for the quantification of Oxcarbazepine (O...

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Section: Development and Validation Of Lc-ms/ms Methods For The Quantimentioning

confidence: 99%

“…The analyst should establish the effects of random events on the precision of the analytical procedure. The intermediate precision is obtained when multiple analysts, using multiple columns, on multiple days in one laboratory, 15,16) perform the assay. In order to study these effects simultane-32…”

Section: Intermediate Precision/ruggednessmentioning

confidence: 99%

Development and Validation of LC-MS/MS Method for the Quantification of Oxcarbazepine in Human Plasma Using an Experimental Design

Gedela

Ratnam

Rao

et al. 2008

CHEMICAL & PHARMACEUTICAL BULLETIN

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“…It is also used for the treatment of moderate to severe restless legs syndrome [1]. Various analytical methods have been reported in literature for determination of pramipexole dihydrochloride, including high performance liquid chromatography (HPLC) [2][3][4][5][6][7][8][9][10][11][12], high performance thin layer chromatography [13], liquid chromatography tandem mass spectrometry [14,15], gas chromatography mass spectrometry GC/MS [16], spectrophotometry [17][18][19][20][21][22][23][24], and potentiometry [25,26]. Recently, voltammetric determination of this drug using glassy carbon electrodes was reported [27][28][29][30].…”

Section: Introductionmentioning

confidence: 99%

Differential Pulse Anodic Voltammetric Determination of the Pharmaceutical Compound Pramipexole Dihydrochloride in its Tablets

Zayed¹,

Oraby²,

Thobety³

et al. 2017

Port. Electrochim. Acta

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The electrochemical behavior of pramipexole dihydrochloride was studied at carbon paste electrodes in 0.04 M Britton-Robinson buffer of pH 6.08, using cyclic and differential pulse voltammetric techniques. The oxidation of pramipexole dihydrochloride is an irreversible diffusion-controlled process. A differential pulse anodic voltammetric procedure has been developed for determination of the drug over the concentration range of 1.20 -8.23 μg/mL, with detection and quantification limits of 0.21 and 0.68 μg/mL, respectively. The proposed method was successfully applied for the determination of the drug in its commercial tablets.

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“…Those methods are based on spectrophotometry (Armağan, 2011;Babu, Raju, 2007;El-Bayoumi, 2009;Gurupadayya, Vishwajith, Srujana, 2009;Rani, Reddy, 2006;Rani, Reddy, 2007;Thangabalan et al, 2011a,b), high-performance liquid chromatography (HPLC) (El-Sherif, Abdel-Fattah, El-Houssini, 2008;Hua et al, 2011;Jancic et al, 2007a,b;Kamienska-Duda, Kosmacinska, 2008;Malenovic et al, 2010;Manish et al, 2010;Ramakrishna et al, 2007;Rao et al, 2009;Shuhui, 2010;Srinubabu et al, 2006;Syeda et al, 2010;Vijaya et al, 2009), gas chromatography (Panchal, Patel, Menon, 2011), and capillary electrophoresis (Musenga et al, 2008;Chang-Hai et al, 2009).…”

Section: Introductionmentioning

confidence: 99%

Validation of high performance liquid chromatographic and spectrophotometric methods for the determination of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products

Sevim

Erk

2015

Braz. J. Pharm. Sci.

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The antiparkinson agent pramipexole dihydrochloride monohydrate was quantified in pharmaceutical products by high performance liquid chromatography (HPLC) and derivative spectrophotometry. The first method was based on HPLC using tamsulosin HCl as an internal standard. In this method, chromatographic separation was achieved using a LiChrospher 60 RP column at 25°C, with a flow rate of 1.0 mL/min at 263 nm. The eluent comprised 0.01 mol/L ammonium acetate (pH 4.4) and acetonitrile (35:65 by volume). The linearity range was found to be 10.0-30.0 µg/mL with a mean recovery of 100.5 ± 1.10. The limit of detection (8 ng/mL) and limit of quantification (50 ng/mL) were calculated. In the second method, the first derivative spectrophotometric technique for the determination of pramipexole dihydrochloride monohydrate was performed by measuring the amplitude at 249 and 280 nm. In the first derivative technique, the absorbance and concentration plot was rectilinear over the 5.0-35.0 µg/mL range with a lower detection limit of 1.5 ng/mL and quantification limit of 4.5 ng/mL. The typical excipients included in the pharmaceutical product do not interfere with the selectivity of either method. The developed methods were validated for robustness, selectivity, specificity, linearity, precision, and accuracy as per the ICH and FDA guidelines (ICH Q2B, 1996; FDA,2000). In conclusion, the developed methods were successful in determining the quantity of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products. The RSD values for the pharmaceutical product used in this study were found to be 0.97% for the HPLC method and 0.00% for the first derivative spectrophotometric method. O fármaco antiparkinsoniano, dicloridrato de pramipexol monoidratado, foi quantificado no produto farmacêutico por cromatografia líquida de alta eficiência (CLAE) e espectrofotometria derivada. No primeiro método baseado na CLAE, o cloridrato de tansulosina foi usado como padrão interno. Nesse método, a separação cromatográfica foi realizada usando uma coluna Lichrosper 60 RP a 25 °C e acetato de amônio 0,01 mol/L (pH:4.4): acetonitrila (35:65 em volume) como eluente com fluxo de 1,0 mL /min a 263 nm. A faixa de linearidade foi de 10.0-30.0 µg/mL com média da recuperação 100.5 ± 1.10. O limite de detecção (8 ng/mL) e o limite de quantificação (50 ng/mL) foram calculados. Por outro lado, a primeira técnica de espectrofotometria derivada para a determinação de dicloridrato de pramipexol monoidratado foi realizada através da medida da amplitude a 249 e 280 nm. Na técnia da primeira derivada, a absorvância e a plotagem da concentração foi retilínea na faixa de 5.0-35.0 µg/mL com limite inferior de detecção de 1.5 ng/mL e limite de quantificação de 4.5 ng/mL. Os excipientes típicos incluídos no produto farmacêutico não interferem com a seletividade dos métodos. Os métodos desenvolvidos foram validados quanto à robustez, seletividade, especificidade, linearidade, precisão e S. Sevim, N. Erk 880 exatidão de acordo com as diretrizes d...

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Development and Validation of a LC Method for the Determination of Pramipexole Using an Experimental Design

Cited by 35 publications

References 13 publications

Development and Validation of LC-MS/MS Method for the Quantification of Oxcarbazepine in Human Plasma Using an Experimental Design

Development and Validation of LC-MS/MS Method for the Quantification of Oxcarbazepine in Human Plasma Using an Experimental Design

Differential Pulse Anodic Voltammetric Determination of the Pharmaceutical Compound Pramipexole Dihydrochloride in its Tablets

Validation of high performance liquid chromatographic and spectrophotometric methods for the determination of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products

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