Development and validation of a HPLC method for the determination of voriconazole in pharmaceutical formulation using an experimental design

Gedela, Srinubabu; Raju, Ch. A. I.; Sarath, N.; Kumar, Pawan; Rao, J. V. L. N. Seshagiri

doi:10.1016/j.talanta.2006.04.042

Cited by 77 publications

(39 citation statements)

References 11 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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“…Intermediate precision is established when the proposed analysis is performed by multiple analysts, using multiple instruments, on multiple days in one laboratory [24]. Hence, it is important for the analyst to identify the effects of random changes/events on method precision [28][29][30]. In the present study, intermediate precision was studied using experimental design methodology.…”

Section: Tablementioning

confidence: 99%

Developing and optimizing a validated isocratic reversed-phase high-performance liquid chromatography separation of nimodipine and impurities in tablets using experimental design methodology

Barmpalexis

Kanaze

Georgarakis

2009

Journal of Pharmaceutical and Biomedical Analysis

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“…[16,17] The analyst should establish the effects of random events on the precision of the analytical procedure. The intermediate precision is obtained when 198 M. H. Semreen and H. Y. Aboul-Enein the assay is performed by multiple analysts, using multiple instruments, on multiple days, in one laboratory.…”

Section: Intermediate Precisionmentioning

confidence: 99%

Experimental Design Strategies in Lc Method Development and in Robustness Testing for Reversible Cholinesterase Inhibitor Rivastigmine in Pharmaceutical Formulation

Semreen

Aboul‐Enein

2009

Journal of Liquid Chromatography & Related Technologies

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& An isocratic, reversed phase liquid chromatographic (RPLC) method was developed for the quantitative determination of rivastigmine hydrogen tartrate, in bulk drugs and in pharmaceutical formulation. The chromatographic separation was achieved on A Vertex Hypersil reversed phase C 18 column (25 cm Â 4.6 mm i.d., particle size 5 lm) using acetonitrile and phosphate buffer. The procedure was validated by linearity (correlation coefficient ¼ 0.9983), accuracy, robustness, and intermediate precision. An experimental design was used during validation to calculate method robustness and intermediate precision. For the robustness test, three factors were considered: percentage v=v of acetonitrile, flow rate, and temperature; an increase in flow rate results in decrease of the concentration of the drug from the expected value, while the percentage of organic modifier and temperature have no effect on the response. For intermediate precision measurement, the considered variables were analyst, equipment, and days. The RSD value (1.10 %, n ¼ 24) indicate a good precision.

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Development and validation of a HPLC method for the determination of voriconazole in pharmaceutical formulation using an experimental design

Cited by 77 publications

References 11 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

Developing and optimizing a validated isocratic reversed-phase high-performance liquid chromatography separation of nimodipine and impurities in tablets using experimental design methodology

Experimental Design Strategies in Lc Method Development and in Robustness Testing for Reversible Cholinesterase Inhibitor Rivastigmine in Pharmaceutical Formulation

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