High-performance liquid chromatographic determination of bromazepam in human plasma

Hirayama, Haruo; Kasuya, Yasuji; Suga, Tetuya

doi:10.1016/s0378-4347(00)84868-9

Cited by 13 publications

(3 citation statements)

References 5 publications

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“…A mobile phase composed of methanol: water (70:30 v/v) was used, with retention times of 4.397, and 5.317 min for BMZ and ABP respectively, Fig 2. The total run time required for the analyses of all the compounds of interest was determined to be approximately 6 min. The required short analysis time may have the added advantage of providing a more rapid method for routine analysis of the main investigated drug, with a great level of accuratness and selectivity when compared to previously reported methods [18,19]. Calibration curves for BMZ and ABP were created by drawing the relative peak area against their correspondant concentration.…”

Section: Hplc Resultsmentioning

confidence: 99%

“…These reported methods also reveal many analytical techniques for BMZ determination either alone or together with other benzodiazepines, in both pharmaceutical or biological matrices. These techniques include HPLC [13][14][15][16][17][18][19][20][21][22][23][24], LC-MS [25,26], GC-MS [27], TLC [28], capillary electrophoresis [29], spectrophotometry [30][31][32], ion-selective electrode [33][34][35], potentiometric [36] and voltammetric [37,38] methods.…”

Section: Introductionmentioning

confidence: 99%

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Development and validation of a stability indicating RP-HPLC-DAD method for the determination of bromazepam

Darwish

Ali²,

Naguib

et al. 2021

PLoS ONE

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A reliable, selective and sensitive stability-indicating RP-HPLC assay was established for the quantitation of bromazepam (BMZ) and one of the degradant and stated potential impurities; 2-(2-amino-5-bromobenzoyl) pyridine (ABP). The assay was accomplished on a C18 column (250 mm × 4.6 mm i.d., 5 μm particle size), and utilizing methanol-water (70: 30, v/v) as the mobile phase, at a flow rate of 1.0 ml min-1. HPLC detection of elute was obtained by a photodiode array detector (DAD) which was set at 230 nm. ICH guidelines were adhered for validation of proposed method regarding specificity, sensitivity, precision, linearity, accuracy, system suitability and robustness. Calibration curves of BMZ and ABP were created in the range of 1–16 μg mL-1 with mean recovery percentage of 100.02 ± 1.245 and 99.74 ± 1.124, and detection limit of 0.20 μg mL-1 and 0.24 μg mL-1 respectively. BMZ stability was inspected under various ICH forced degradation conditions and it was found to be easily degraded in acidic and alkaline conditions. The results revealed the suitability of the described methodology for the quantitation of the impurity (ABP) in a BMZ pure sample. The determination of BMZ in pharmaceutical dosage forms was conducted with the described method and showed mean percentage recovery of 99.39 ± 1.401 and 98.72 ± 1.795 (n = 6), respectively. When comparing the described procedure to a reference HPLC method statistically, no significant differences between the two methods in regard to both accuracy and precision were found.

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Section: Hplc Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Development and validation of a stability indicating RP-HPLC-DAD method for the determination of bromazepam

Darwish

Ali²,

Naguib

et al. 2021

PLoS ONE

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“…In clinical and forensic toxicology, several chromatographic methods have been described for the determination of bromazepam in human biosamples (whole blood, plasma or serum), including gas/liquid chromatography coupled to electron‐capture detection (GLC/ECD),3 gas chromatography coupled to electron‐capture detection (GC/ECD),4, 5 high‐performance liquid chromatography coupled to UV detection (HPLC/UV),6–15 gas chromatography coupled to mass spectrometry (GC/MS),16–18 gas chromatography coupled to tandem mass spectrometry (GC/MS/MS)19 and liquid chromatography coupled to mass spectrometry (LC/MS) 20, 21. Chromatographic techniques are commonly used to quantify bromazepam in a specimen initially screened by a immunoassay‐based method 22…”

Section: Introductionmentioning

confidence: 99%

Bromazepam determination in human plasma by high‐performance liquid chromatography coupled to tandem mass spectrometry: a highly sensitive and specific tool for bioequivalence studies

Laurito¹,

Mendes²,

Santagada³

et al. 2004

J. Mass Spectrom.

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A rapid, sensitive and specific method to quantify bromazepam in human plasma using diazepam as the internal standard (IS) is described. The analyte and the IS were extracted from plasma by liquid-liquid extraction using diethyl ether-hexane (80 : 20, v/v). The extracts were analyzed by high-performance liquid chromatography (HPLC) coupled to electrospray tandem mass spectrometry (MS/MS). Chromatography was performed isocratically on a Genesis C(18) analytical column (100 x 2.1 mm i.d., film thickness 4 microm). The method had a chromatographic run time of 5.0 min and a linear calibration curve over the range 5.0-150 ng ml(-1) (r(2) > 0.9952). The limit of quantification was 5 ng ml(-1). This HPLC/MS/MS procedure was used to assess the bioequivalence of two bromazepam 6 mg tablet formulations (bromazepam from Medley SA Indústria Farmacêutica as the test formulation and Lexotan from Produtos Roche Químico e Farmacêutico SA as the reference formulation). A single 6 mg dose of each formulation was administered to 24 healthy volunteers (12 males and 12 females). The study was conducted using an open, randomized, two-period crossover design with a 3 week washout interval. Since the 90% CI for C(max), AUC(last), AUC(0-240 h) (linear) and AUC((0- infinity )) ratios were all inside the 80-125% interval proposed by the US Food and Drug Administration, it was concluded that the bromazepam formulation from Medley is bioequivalent to the Lexotan formulation for both the rate and the extent of absorption.

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Determination of bromazepam in human plasma by high‐performance liquid chromatography with electrospray ionization tandem mass spectrometric detection: application to a bioequivalence study

Andraus

Wong²,

Silva³

et al. 2004

J. Mass Spectrom.

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A simple method using a one-step liquid-liquid extraction (LLE) followed by high-performance liquid chromatography (HPLC) with positive ion electrospray ionization tandem mass spectrometric (ESI-MS/MS) detection was developed for the determination of bromazepam in human plasma, using lorazepam as internal standard. The acquisition was performed in the multiple reaction monitoring mode, monitoring the transitions: m/z 316 > 182 for bromazepam and m/z 321 > 275 for lorazepam. The method was linear over the studied range (1-100 ng ml(-1)), with r(2) > 0.98, and the run time was 2.5 min. The intra- and inter-assay precisions were 2.7-14.6 and 4.1-17.3%, respectively and the intra- and inter-assay accuracies were 87-111 and 75.8-109.5%, respectively. The mean recovery was 73.7%, ranging from 64.5 to 79.7%. The limit of quantification was 1 ng ml(-1). At this concentration the mean intra- and inter-assay precisions were 14.6 and 7.1%, respectively, and the mean intra- and inter-assay accuracies were 102.5 and 104%, respectively. Bromazepam stability was evaluated and the results showed that the drug is stable in standard solution and in plasma samples under typical storage and processing conditions. The method was applied to a bioequivalence study in which 27 healthy adult volunteers (14 men) received single oral doses (6 mg) of reference and test bromazepam formulations, in an open, two-period, randomized, crossover protocol. The 90% confidence interval of the individual ratios (test formulation/reference formulation) for C(max) (peak plasma concentration), AUC(0-96) and AUC(0-inf) (area under the plasma concentration versus time curve from time zero to 96 h and to infinity, respectively) were within the range 80-125%, which supports the conclusion that the test formulation is bioequivalent to the reference formulation regarding the rate and extent of bromazepam absorption.

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High-performance liquid chromatographic determination of bromazepam in human plasma

Cited by 13 publications

References 5 publications

Development and validation of a stability indicating RP-HPLC-DAD method for the determination of bromazepam

Development and validation of a stability indicating RP-HPLC-DAD method for the determination of bromazepam

Bromazepam determination in human plasma by high‐performance liquid chromatography coupled to tandem mass spectrometry: a highly sensitive and specific tool for bioequivalence studies

Determination of bromazepam in human plasma by high‐performance liquid chromatography with electrospray ionization tandem mass spectrometric detection: application to a bioequivalence study

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