Validated HPLC–MS/MS method for simultaneous determination of simvastatin and simvastatin hydroxy acid in human plasma

Barrett, B.; Huclová, Jitka; Bořek-Dohalský, V.; Němec, B.; Jelı́nek, Ivan

doi:10.1016/j.jpba.2005.11.020

Cited by 60 publications

(39 citation statements)

References 16 publications

(18 reference statements)

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“…Simvastatin is orally administered as inactive prodrug in the lactone form which is converted in the liver into its active metabolite β-hydroxy acid [3]. Recently, numerous methods for analysis of simvastatin and its metabolites determination in human plasma by HPLC methods with difference detectors (ultraviolet, fluorescence and mass spectrometry) have been published [4][5][6][7][8][9]. In addition, some methods of gas chromatography with mass spectrometry for determination of simvastatin and its metabolites have also been published [10][11].…”

Section: Introductionmentioning

confidence: 99%

“…Therefore, sensitive and selective methods for the determination of simvastatin are required for therapeutic drug level monitoring. A more sensitive method using LC/MS/MS, can be achieved, but the operation and clean up procedure prior to analysis seems to be so complicated and is too expensive to be used for routine measurements in the clinical laboratory [6,8,9]. Electrospray ionization mass spectrometry (ESI-MS) coupled with LC-MS method developed by Yang et al, (2003) was simple, rapid and sensitive.…”

Section: Introductionmentioning

confidence: 99%

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Method Validation for Analysis of Simvastatin in Human Plasma Using Liquid Chromatography Tandem Mass Spectrometry (LC-MS-MS)

Alakhali¹

2013

JCDR

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Introduction: The Liquid Chromatography Tandem Mass Spectrometry (LC-MS-MS) for determination simvastatin in human plasma has been developed after extraction by by ethyl acetate and hexane (90/10%, v/v) using lovastatin as internal standard. Material and Methods:The mobile phase consisting of mixture of acetonitrile and water (75/25%, v/v) 500μL/min by separated the solutes on a C18 column. discussion:The lower limit of quantitation of 0.25 ng/mL was achieved when the calibration curve was linear from 0.25-50 ng/mL. The entire run time for analysis was only 6 min. The quantitation in the selective reaction monitoring (SRM) in positive ion mode, the daughter ions m/z 325 for simvastatin and m/z 285 for lovastatin were used. The Parent ions in positive ion mode were m/z 441.3 for simvastatin and m/z 405.1 for lovastatin. The intra-day coefficients of variation were less than 14% while the inter-day coefficients of variation were less than 10%. conclusion:The LC-MS-MS detection is sensitive due to its capability to eliminate interferences from endogenous components.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Method Validation for Analysis of Simvastatin in Human Plasma Using Liquid Chromatography Tandem Mass Spectrometry (LC-MS-MS)

Alakhali¹

2013

JCDR

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“…Following conversion of this lactone prodrug to its hydroxyl acid form, the compound is a potent competitive inhibitor of HMGCoA reductase, the rate limiting enzyme in cholesterol biosynthesis 2 . Different analytical methods have been reported for the determination of simvastatin, which include HPLC [3][4][5][6] , HPLC-MS/MS 7 , derivative spectrophotometry 8 and Voltammetric techniques 9 .…”

Section: Simvastatin (Fig 1) a Hypolipidemic Drug Belonging To The mentioning

confidence: 99%

HPLC Determination of Ezetimibe and Simvastatin in Pharmaceutical Formulations

Ashfaq

Ullahkhan

Qutab³

et al. 2007

J. Chil. Chem. Soc.

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A simple, precise and sensitive reverse-phase high performance liquid chromatographic method was developed and validated for the simultaneous determination of ezetimibe and simvastatin in pharmaceutical formulations. Chromatographic separation was performed on a Merck C18 column at a wavelength of 240 nm using a mixture of 0.1M ammonium acetate buffer pH 5.0 and acetonitrile in the ratio of (30:70, v/v). The method results in excellent separation with good resolution between the two analytes. The within day variation was between 0.28 and 1.10 % and between day variation was between 0.56 and 1.32 %. The recovery was greater than 99.12 % with RSD less than 1.38 %. The method was validated according to ICH guidelines by performing linearity, accuracy, precision, limits of quantitation and selectivity. The results show that the method is suitable for its intended use.

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“…These procedures include spectrophotometric comprising simultaneous determination of EZE and atorvastatin calcium in pharmaceutical dosage form [3], also, simvastatin and fluvastatin in human plasma and pharmaceutical formulation [4], TLC [5][6][7], LC [3,[8][9][10][11][12][13][14][15][16][17][18][19][20][21][22][23][24][25][26], Capillary Zone Electrophoresis (CZE) [27,28] and GC [29] methods.…”

Section: Introductionmentioning

confidence: 99%

Derivative spectrophotometric method for simultaneous determination of ezetimibe and simvastatin in combined tablets

2010

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KEYWORDSThe introduced study portrays the development and validation of an effortless, speedy and selective first order derivative zero-crossing spectrophotometric method to estimate ezetimibe and simvastatin simultaneously in combined drug products over and above in the presence of ezetimibe alkaline degradation products. Ezetimibe and its alkaline degradates spectra showed zero-crossing point at 249 nm, so the amplitude at 249 nm could be used for calculating the concentration of simvastatin. While simvastatin and ezetimibe alkaline degradates spectra showed a zero-reading value at 261 nm, so ezetimibe could be determined by measuring the amplitude at 261 nm. Regression plots revealed good linear relationships in the concentration range 1-16 µg/mL with accuracy checked by conducting recovery studies; average recovery was 99.61 ± 1.183 and 100.47 ± 1.310 for ezetimibe and simvastatin, respectively. The suggested first derivative spectrophotometric method was successfully applied for the determination of the cited drugs in "Inegy 10/10, 10/20 and 10/40 tablets". Satisfactory results were obtained for the recovery of both drugs and were in good agreement with the labeled amounts. Method validation was estimated according to USP guidelines.

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Validated HPLC–MS/MS method for simultaneous determination of simvastatin and simvastatin hydroxy acid in human plasma

Cited by 60 publications

References 16 publications

Method Validation for Analysis of Simvastatin in Human Plasma Using Liquid Chromatography Tandem Mass Spectrometry (LC-MS-MS)

Method Validation for Analysis of Simvastatin in Human Plasma Using Liquid Chromatography Tandem Mass Spectrometry (LC-MS-MS)

HPLC Determination of Ezetimibe and Simvastatin in Pharmaceutical Formulations

Derivative spectrophotometric method for simultaneous determination of ezetimibe and simvastatin in combined tablets

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