SEPARATION AND DETERMINATION OF Β-Lactamase INHIBITORS IN HUMAN SERUM BY HPLC WITH a Β-Cyclodextrin STATIONARY PHASE

Tsou, Tai Li; Wu, Jing-Ran; Tang, Shang-Tao; Liu, Hwan-Wun

doi:10.1081/jlc-120016212

Cited by 6 publications

(8 citation statements)

References 36 publications

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“…The poor retention of clavulanic acid (p K a = 2.7) on a reversed‐phase column has already been published in the literature. Generally nonvolatile ion‐pairing reagents such as tri‐ and tetra‐alkylammonium salts4–7, 10, 11, 21, 22 and phosphate buffers8, 9, 12–16 are used in the mobile phase to lengthen the retention time, but these are not recommended for use in LC‐MS/MS. These compounds would precipitate in the LC‐MS interface, contaminate the ionization source and may cause ion suppression 34.…”

Section: Resultsmentioning

confidence: 99%

“…Nevertheless, during the last decades, a lot of chromatographic assays were developed for the determination of clavulanic acid in plasma and urine. However, ultraviolet (UV) detection4–7 of clavulanic acid in biological matrices is difficult because of the low detection wavelength and consequently owing to the presence of endogenous compounds absorbing at this wavelength. Therefore, several methods make use of a precolumn derivatization with imidazole4, 8–13 or triazole14–16 combined with UV‐detection or fluorimetric detection after derivatization with benzaldehyde 17.…”

Section: Introductionmentioning

confidence: 99%

“…Hoizey et al 4 used methanol for the deproteinization of plasma. However, some authors described a reduced stability of clavulanic acid in methanol 6, 28. In this paper, the stability of clavulanic acid is thoroughly tested according to the Guidelines for Bioanalytical Method Validation of The Food and Drug Administration (FDA) including: freeze and thaw stability, short‐term temperature stability, long‐term temperature stability, stock solution stability and postpreparative stability 29…”

Section: Introductionmentioning

confidence: 99%

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Determination of clavulanic acid in calf plasma by liquid chromatography tandem mass spectrometry

et al. 2006

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A method for the quantification of clavulanic acid in calf plasma using high-performance liquid chromatography combined with electrospray ionization (ESI) mass spectrometry, operating in the negative ionization mode (LC-MS/MS), is presented. Sample preparation includes a simple and fast deproteinization with acetonitrile and a back-extraction of the acetonitrile with dichloromethane. Chromatography is performed on a reversed-phase PLRP-S polymeric column using 0.05% formic acid in water and acetonitrile. The limit of quantification is 25 ng/ml, which is lower than other published methods using ultraviolet (UV), fluorimetric or mass spectrometric detection. The limit of detection is calculated to be 3.5 ng/ml. The stability of clavulanic acid was demonstrated according to The Guidelines of Bioanalytical Method Validation of The Food and Drug Administration (FDA): freeze and thaw stability, short-term stability, long-term stability, stock solution stability and postpreparative stability. The method is used in a pharmacokinetic and bioequivalence study of amoxycillin/clavulanic acid formulations in calves.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Determination of clavulanic acid in calf plasma by liquid chromatography tandem mass spectrometry

et al. 2006

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“…A deproteinization in MEOH, acidic, or basic medium is unsuitable as it is well-known that CLV is unstable in MEOH (Tsou et al 2002), acidic, and basic conditions (Foulstone and Reading 1982). These results were also proven by our experiments.…”

Section: Sample Preparationmentioning

confidence: 99%

Simultaneous Determination of Amoxicillin and Clavulanic Acid in Dog Plasma by High-Performance Liquid Chromatography Tandem Mass Spectrometry

Guo

et al. 2012

Analytical Letters

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A rapid, sensitive, and specific high-performance liquid chromatography tandem mass spectrometric method was developed for the simultaneous determination and confirmation of amoxicillin and clavulanic acid in plasma. Plasma sample was subjected to a simple deproteinization with acetonitrile, and then the supernatant was directly diluted by water. Analysis was performed on a Phenomenex Luna C 8 reversed-phase column by detection with mass spectrometry in negative ions multiple reaction monitoring mode. A gradient elution program with 0.1% formic acid and acetonitrile was performed at a flow of 0.25 mL min À1 . There is good linearity in the range of 0.5-500 ng mL À1 for both amoxicillin and clavulanic acid. The decision limits of amoxicillin and clavulanic acid were 0.06 ng mL À1 and 0.08 ng mL À1 in plasma, respectively, and the detection capabilities of two analytes were below 0.5 ng mL À1 . Acceptable precision and accuracy were obtained for concentrations over the standard curve range. The extraction recoveries of amoxicillin and clavulanic acid were between 102% and 115% in plasma at three spiked levels of 0.5, 50, and 500 ng mL À1 , with the relative standard deviations less than 15% for each analyte. The developed method was applied to pharmacokinetic studies of amoxicillin and clavulanic acid tablets in healthy beagles.

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“…Several β-lactamase inhibitors have been developed against the target enzyme. 11 When they are combined with some penicillins or cephalosporins, the mixed ingredients have been shown to be effective against various β-lactamase producing bacteria both in vitro and in vivo. [12][13][14][15] Various methods are available for the analysis of TZB in biological samples [16][17][18] or in pharmaceutical formulations [19][20][21] in combination with different drugs by high performance liquid chromatography (HPLC).…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Determination of Cefepime and Tazobactam in Injectables by Ultra-High Performance Liquid Chromatography Method

Shrestha¹,

Bhuyan²,

Sinha³

2014

Phm

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Aim: Stability indicating ultra-high performance liquid chromatography (UHPLC) method was developed and validated for the determination of cefepime (CFPM) and tazobactam (TZB) in injectable dosage form. Materials and Methods: Separation was performed in a Dionex Ultimate 3000 UHPLC system equipped with chromeleon software using Acclaim 120 C 18 (250 × 4.6 mm, 5 μm particle size) column with mobile phase (pH 6.0) containing methanol and sodium acetate buffer in the ratio of 11:89 v/v with a fl ow rate of 1.8 mL/min and detection wavelength of 220 nm. Stress studies were performed using HCl, NaOH, H 2 O 2 , and ultraviolet radiation. Results: The method was found to be linear in the concentration range of 50-350 μg/ml (R 2 = 0.998) and 6.25-43.75 μg/ml (R 2 = 0.998) with the regression equation y = 11068 x + 115231 and y = 8317.1x-9869.7 for CFPM and TZB, respectively. The percentage of relative standard deviation (%RSD) of 0.63 and 1.39 for intra-day and 0.64 and 0.54 for inter-day precision, respectively for CFPM and TZB suggest the precision of the method as all these values are <2%. It was found from the stress studies that both the drugs are very susceptible to alkaline condition. The method has shown good, consistent recoveries for CFPM (100.6-102.0%) with mean RSD of 0.73% and TZB (98.4-100.6%) with mean RSD of 1.14%, which indicates the method is suffi ciently accurate. Conclusion: The method was found to be accurate, precise, specifi c, robust, linear, and stability indicating for the determination of CFPM and TZB in injectable dosage form.

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SEPARATION AND DETERMINATION OF Β-Lactamase INHIBITORS IN HUMAN SERUM BY HPLC WITH a Β-Cyclodextrin STATIONARY PHASE

Cited by 6 publications

References 36 publications

Determination of clavulanic acid in calf plasma by liquid chromatography tandem mass spectrometry

Determination of clavulanic acid in calf plasma by liquid chromatography tandem mass spectrometry

Simultaneous Determination of Amoxicillin and Clavulanic Acid in Dog Plasma by High-Performance Liquid Chromatography Tandem Mass Spectrometry

Simultaneous Determination of Cefepime and Tazobactam in Injectables by Ultra-High Performance Liquid Chromatography Method

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