Fast high performance liquid chromatography method for in-process control of sulbactam

Gomis, Domingo Blanco; Núñez, Noé Sánchez; García, Eliseo; Bayod, Miguel; Álvarez, Manuel

doi:10.1016/j.aca.2003.08.046

Cited by 6 publications

(3 citation statements)

References 17 publications

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“…There are also a few papers referring to the determination of the impurities in the active pharmaceutical ingredients (API) of bosentan monohydrate and compounds generated during the degradation study [1, 19, 20]. Some papers deal with the analysis of the in-process control (IPC) of the API [21, 22]; however, there is no uniform requirement to follow the guidelines for the IPC methods.…”

Section: Introductionmentioning

confidence: 99%

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Development and Validation of a UHPLC UV Method for the In-Process Control of Bosentan Monohydrate Synthesis

et al. 2016

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Bosentan monohydrate (4-tert-butyl-N-[6-(2-hydroxyethoxy)-5-(2-methoxyphenoxy)-2-(pyrimidin-2-yl) pyrimidin-4-yl]benzene-1-sulfonamide monohydrate) is a dual endothelin receptor antagonist (ERA) applied in the treatment of pulmonary arterial hypertension. To achieve effective process control of the bosentan monohydrate synthesis, it was necessary to develop a selective and not highly time-consuming method for ultra-high performance liquid chromatography (UHPLC). The method is characterized by adequate sensitivity, reproducibility and selectivity for the determination of bosentan monohydrate and related compounds from all synthetic stages. The UHPLC separation was carried out by reversed phase chromatography on the Acquity BEH C18 column (100 mm × 2.1 mm, 1.7 µm) with a mobile phase composed of solvent A (0.1 %, v/v, acetic acid in water) and solvent B (methanol), in the gradient mode at the flow rate of 0.4 mL min−1. Limits of detection and quantification for the compounds were ≤0.1 µg mL−1 and 0.3 µg mL−1, respectively. The linearity for all related compounds was investigated as in the range for the active pharmaceutical ingredient (API) and as in the range for the in-process control. The developed method was validated according to the current guidelines, proving the suitability of the method for its intended purpose.

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Section: Introductionmentioning

confidence: 99%

“…The analytical procedure was published in the authorized USP Pending Monograph and in the United States Pharmacopeia Convention. It recommends applying HPLC UV for the determination of bosentan monohydrate and related substances [20, 21]. …”

Section: Introductionmentioning

confidence: 99%

Development and Validation of a UHPLC UV Method for the In-Process Control of Bosentan Monohydrate Synthesis

et al. 2016

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“…Several studies have reported various analytical methods for the determination of sulbactam in pharmaceutical formulations (Mahgoub and Aly, 1998;Aly et al, 2000;Pajchel et al, 2002;Blanco Gomis et al, 2003;Dinç and Baleanu, 2006;Hoang et al, 2014;Marwada et al, 2014) and human plasma and serum (Guillaume et al, 1995;Aly et al, 2000;Carlier et al, 2012); however, few methods have been developed for the determination of sulbactam in foodstuff (Li et al, 2014). The methods reported in previous studies included capillary electrophoresis (Pajchel et al, 2002), UV spectrophotometry (Mahgoub and Aly, 1998;Hoang et al, 2014;Marwada et al, 2014), fractional wavelet transform (Dinç and Baleanu, 2006), chemiluminometric (Aly et al, 2000), HPLC (Guillaume et al, 1995;Blanco Gomis et al, 2003), and ultra-highperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS; Carlier et al, 2012;Li et al, 2014). Although the method outlined by Li and colleagues (2014) had been reported to determine sulbactam in bovine milk, we still hoped to optimize the mentioned method to achieve better performance by (1) using organic solvents in our study to extract analytes and precipitate proteins without adjusting the pH value of the extraction solution; (2) lowering the method's detection limit than the previous study by replacing high volumes of elute with lower volumes of solvent after an solid-phase extraction (SPE) procedure; or (3) applying the isotope dilution method to the quantitative analysis so that the analysis in a complex matrix could overcome difficulties.…”

Section: Introductionmentioning

confidence: 99%

Determination of sulbactam in raw bovine milk by isotope dilution–ultra-high-performance liquid chromatography–tandem mass spectrometry

Zhang

et al. 2019

Journal of Dairy Science

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We developed a sensitive and selective isotope dilution ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the determination of sulbactam residue in raw bovine milk. Sulbactam and internal standard, sulbactam-d 5 , were extracted from raw bovine milk via liquid-liquid extraction and enriched with strong anion exchange solid-phase extraction cartridges and finally analyzed by using UPLC-MS/MS with multiple reaction monitoring mode. The method was validated according to European regulations. The calibration curve showed good linearity, with a correlation coefficient of 0.9998. Decision limit and detection capability of sulbactam were determined by matrix calibration curve and were 0.0445 and 0.0517 μg/L, respectively. The recoveries of sulbactam in fortified raw bovine milk ranged from 72.1 to 91.5%, with the intra-and interday relative standard deviations ranging from 3.0 to 18.9%. Furthermore, the developed method was applied to analyzing real raw bovine milk samples collected from dairy farms in Beijing, China. Sulbactam was not determined in all samples. The proposed method could ultimately serve as a methodological foundation for the determination of sulbactam in different types of raw milk and dairy products.

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Ultraviolet spectrophotometry (dual wavelength and chemometric) and high performance liquid chromatography for simultaneous estimation of meropenem and sulbactam sodium in pharmaceutical dosage form

Marwada

Patel

et al. 2014

Spectrochimica Acta Part A: Molecular and Biomolecular Spectros

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Fast high performance liquid chromatography method for in-process control of sulbactam

Cited by 6 publications

References 17 publications

Development and Validation of a UHPLC UV Method for the In-Process Control of Bosentan Monohydrate Synthesis

Development and Validation of a UHPLC UV Method for the In-Process Control of Bosentan Monohydrate Synthesis

Determination of sulbactam in raw bovine milk by isotope dilution–ultra-high-performance liquid chromatography–tandem mass spectrometry

Ultraviolet spectrophotometry (dual wavelength and chemometric) and high performance liquid chromatography for simultaneous estimation of meropenem and sulbactam sodium in pharmaceutical dosage form

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