Efficient high-performance liquid chromatographic assay for the simultaneous determination of metoprolol and two main metabolites in human urine by solid-phase extraction and fluorescence detection

Chiu, F.C.K.; Damani, L. A.; Li, R.C; Tomlinson, Brian

doi:10.1016/s0378-4347(97)00059-5

Cited by 32 publications

(26 citation statements)

References 5 publications

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“…Pharmacokinetic parameters obtained using the proposed method are in agreement with those of the studies reported previously [3,8]. Furthermore, low volumes of plasma and urine (0.5 mL) are used in the proposed method, which can be advantageous in clinical pharmacokinetic studies.…”

Section: Applicationsupporting

confidence: 87%

“…Recovery data are summarized in Table 3. The mean recoveries are better for plasma and urine than those of the studies reported by Albers et al [6], Chiu et al [8] and Johnson et al [11].…”

Section: Recoverymentioning

confidence: 53%

“…The retention time of metoprolol (4.7 min) was quite shorter than that studied by Fang et al [2] and Chiu et al [8]. On the contrary, the mobile phase in the proposed method methanol-water instead of buffered systems is used in previously reported HPLC methods [6,8]. Therefore, flushing of the column after analysis is not required.…”

Section: Methods Development and Optimizationmentioning

confidence: 84%

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Determination of metoprolol in human plasma and urine by high‐performance liquid chromatography with fluorescence detection

Yılmaz

Aşçı

Arslan

2010

J of Separation Science

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A simple, specific and sensitive HPLC method has been developed for the determination of metoprolol in human plasma and urine. Separation of metoprolol and atenolol (internal standard) was achieved on an Ace C(18) column (5 microm, 250 mm x 4.6 mm id) using fluorescence detection with lambda(ex)=276 nm and lambda(em)=296 nm. The mobile phase consists of methanol-water (50:50, v/v) containing 0.1% TFA. The analysis was performed in less than 10 min with a flow rate of 1 mL/min. The assay was linear over the concentration range of 3-200 and 5-300 ng/mL for plasma and urine, respectively. The LOD were 1.0 and 1.5 ng/mL for plasma and urine, respectively. The LOQ were 3.0 and 5.0 ng/mL for plasma and urine, respectively. The extraction recoveries were found to be 95.6 +/- 1.53 and 96.4 +/- 1.75% for plasma and urine, respectively. Also, the method was successfully applied to three patients with hypertension who had been given an oral tablet of 100 mg metoprolol.

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Section: Applicationsupporting

confidence: 87%

“…Recovery data are summarized in Table 3. The mean recoveries are better for plasma and urine than those of the studies reported by Albers et al [6], Chiu et al [8] and Johnson et al [11].…”

Section: Recoverymentioning

confidence: 53%

Section: Methods Development and Optimizationmentioning

confidence: 84%

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Determination of metoprolol in human plasma and urine by high‐performance liquid chromatography with fluorescence detection

Yılmaz

Aşçı

Arslan

2010

J of Separation Science

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“…Balmé r et al 21 achieved a quantitation limit of 14 ng/ml plasma for each isomer. In order to analyze enantiomeric mixture of ␣-hydroxymetoprolol, solid-phase extraction using C-2 for plasma samples 36 or C-18 columns for urine samples 37 obtained high recovery (more than 80.0%) and low quantitation limit (Յ1 ng/ml).…”

Section: Resultsmentioning

confidence: 99%

Stereoselective metabolism of metoprolol: Enantioselectivity of α‐hydroxymetoprolol in plasma and urine

et al. 2003

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Direct stereoselective separation on chiral stationary phase was developed for HPLC analysis of the four stereoisomers of alpha-hydroxymetoprolol in human plasma and urine. Plasma samples were prepared using solid-phase extraction columns and urine samples were prepared by liquid-liquid extraction. The stereoisomers were separated on a Chiralpak AD column at 24 degrees C with fluorescence detection and a mobile phase consisting of a mixture of hexane:ethanol:isopropanol:diethylamine (88:10.2:1.8:0.2) for plasma samples and hexane:ethanol:diethylamine (88:12:0.2) for urine samples. Calibration curves for the individual stereoisomers were linear within the concentration range of 2.0-200 ng/ml plasma or 0.125-25 microg/ml urine. The methods were validated with intra- and interday variations less than 15%. The absolute configuration of the pure stereoisomers were assigned by circular dichroism spectra. The methods were employed to determine the concentrations of alpha-hydroxymetoprolol stereoisomers in a metabolism study of multiple-dose administration of racemic metoprolol to hypertensive patients phenotyped as extensive metabolizers of debrisoquine. We observed stereo-selectivity in the alpha-hydroxymetoprolol formation favoring the new 1'R chiral center from both metoprolol enantiomers (AUC(0-24) (1'R1'S) = 3.02). The similar renal clearances (Cl(R)) of the four stereoisomers demonstrated absence of stereoselectivity in their renal excretion. (-)-(S)-metoprolol was slightly more alpha-hydroxylated than its antipode (AUC(0-24) (2S/2R) = 1.19), suggesting that this pathway is not responsible for plasma accumulation of this enantiomer in humans.

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“…2) Several analytical methods have been developed for the determination of metoprolol in biological fluids and pharmaceutical formulations based on high performance liquid chromatography, [3][4][5][6][7][8][9][10][11] gas chromatography, 12,13) capillary electrophoresis, 14) thin layer chromatography, 15,16) infrared spectroscopy, 17) and electrochemical methods. 18,19) The above mentioned techniques are sensitive but expensive and require laborious clean up procedure prior to analysis.…”

mentioning

confidence: 99%

Validated Kinetic Spectrophotometric Method for the Determination of Metoprolol Tartrate in Pharmaceutical Formulations

Rahman

Azmi

2005

Chem. Pharm. Bull.

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Metoprolol tartrate is a selective b-adrenergic antagonist, which is used in the treatment of cardiovascular disorders such as hypertension, angina pectoris, cardiac arrhythmias and myocardial infarction. The drug is quite sensitive, even a small dose of the drug gives sufficient blockade. Since the bblockers are also misused as doping agents in sports and therefore these drugs have been added to the list of forbidden drugs by the International Olympic Committee (IOC). 1)Therefore the development of an analytical method for the determination of metoprolol tartrate is of great significance.The assay of the drug is listed in the monograph of British Pharmacopoeia, which describes a potentiometric titration method.2) Several analytical methods have been developed for the determination of metoprolol in biological fluids and pharmaceutical formulations based on high performance liquid chromatography, [3][4][5][6][7][8][9][10][11] gas chromatography, 12,13) capillary electrophoresis, 14) thin layer chromatography, 15,16) infrared spectroscopy, 17) and electrochemical methods. 18,19) The above mentioned techniques are sensitive but expensive and require laborious clean up procedure prior to analysis. Spectrophotometry is the technique of choice even today due to its inherent simplicity and therefore frequently used in the laboratories of the developing countries to overcome versatile analytical problem. The drug has been determined in the visible region based on ion-pair formation between drug and reagents like oxidized quercetin 20) ; bromophenol blue, bromocresol purple, bromocresol green ; and carbon disulfide-copper chloride. 24)The charge transfer complexation reactions of metoprolol tartrate with s and p-acceptors 24,25) have also been utilized for its quantification in pharmaceutical formulations. Shingbal and Bhangle 26) have reported a spectrophotometric method based on the reaction of drug with 2,4-dinitrofluorobenzene in HCl/dioxan medium to form a colored chromophore, which absorbs maximally at 380 nm. The quantification of metoprolol tartrate was done on treatment of the drug with ammonium metavanadate, 27) FeCl 3 , 28) N-bromosuccinimide, 29) and a mixture of KNO 3 and H 2 SO 4 followed by addition of alkali to get colored chromophore.30) The literature is still poor in analytical procedures based on kinetic spectrophotometry for the determination of drug in pharmaceutical preparations. There is, therefore, a need for a simple and sensitive kinetic spectrophotometric method for the determination of metoprolol tartrate in pharmaceutical formulations. It was found that potassium permanganate oxidizes the metoprolol in alkaline medium and this reaction has not been used before to quantify the drug spectrophotometrically. This paper describes a simple and sensitive kinetic spectrophotometric method for the determination of metoprolol tartrate in drug formulations. The method involves the oxidation of drug with alkaline potassium permanganate at 25Ϯ1°C and subsequent measurement of absorbance at 610 nm. The in...

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Efficient high-performance liquid chromatographic assay for the simultaneous determination of metoprolol and two main metabolites in human urine by solid-phase extraction and fluorescence detection

Cited by 32 publications

References 5 publications

Determination of metoprolol in human plasma and urine by high‐performance liquid chromatography with fluorescence detection

Determination of metoprolol in human plasma and urine by high‐performance liquid chromatography with fluorescence detection

Stereoselective metabolism of metoprolol: Enantioselectivity of α‐hydroxymetoprolol in plasma and urine

Validated Kinetic Spectrophotometric Method for the Determination of Metoprolol Tartrate in Pharmaceutical Formulations

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