Analysis of Paracetamol Using Solid-Phase Extraction, Deuterated Internal Standards, and Gas Chromatography-Mass Spectrometry (original) (raw)
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Bulletin of Pharmaceutical Sciences, 2023
Etoricoxib is a non-steroidal, anti-inflammatory drug (NSAID) and a selective inhibitor of Cyclooxygenase 2 (COX2), which makes it safer on the gastrointestinal tract than the other NSAIDs. Given the importance of Etoricoxib's, its combination with paracetamol offers higher efficacy and fewer side effects. In addition to the popularity of this combination in the pharmaceutical industry and the diversity of its manufacturing companies, this study aims to develop a novel, precise, selective, rapid and economic assay method for the simultaneous quantitative determination of Etoricoxib and paracetamol in bulk and pharmaceutical dosage form using reverse phase HPLC. This developed method has a short run time of less than 4 minutes using a C18 column (150×4.6) mm 5μm, a mobile phase of methanol and ammonium acetate (pH =3.5) in a ratio (60:40), respectively. The elution was observed at 245 nm using a PDA detector; the retention times of paracetamol and Etoricoxib were found to be 2.493 and 3.64 min, respectively, and a resolution factor larger than 2. Linearity was established with correlation coefficient values of 0.9991, 0.9994 for both Etoricoxib and paracetamol drugs. Precision was within the relative standard deviation of less than 2% for both drugs, and the percentage recoveries were found to be 99.98% and 99.35% for paracetamol and Etoricoxib, respectively. LOD and LOQ of paracetamol were 1.4 g/ml and 4.3 g/ml, respectively, and 0.52 g/ml and 1.6 g/ml for Etoricoxib, respectively. The selectivity test results showed no interference from the tablet excipients during the separation process, which verifies that this method is easily applicable to quality control labs and pharmaceutical industries, in addition to being fast, accurate and cost-effective.
The Dtermination of Paracetamol by HPLC Validation of the Method and Application on Serum Samples
Revista de Chimie
Pain is defined as a disagreeable sensory and emotional experience related to a tissue or potential lesion. Paracetamol (Acetaminophen) is the most used non-morphine analgesic. For the determination of paracetamol we developed and validated the high performance liquid chromatography (HPLC) analysis using a Dionex Ultimate 3000 liquid chromatograph equipped with a multidimensional detector. After determining the optimum conditions of analysis (80/20 water / acetonitrile mobile phase, flow rate 1.0 mL / min, detection wavelength 245 nm) we validated the method following the following parameters: linearity of response function, linearity of results, limit (LD = 0.66 mg / mL) and quantification limit (LQ = 2.00 mg / mL), and precision. The method of determining paracetamol by HPLC was applied to 30 samples of serum collected from patients who had pain and were treated with paracetamol.
Journal of Science and Technology (Ghana), 2006
High Performance Liquid Chromatography has been used to evolve an analytical procedure for the evaluation of the content of paracetamol in the bulk, dosage forms and in urine, a body fluid. Separation and resolution have been achieved with a combination of methanol and 2.5% acetic acid (15:85) on a reversed-phase column at ambient temperature. Elution was isocratic with UV detection at 257nm. Internal standard calibration method was used for quantitation with caffeine as the internal standard. Mean retention times for paracetamol and caffeine were respectively 2.61 ± 0.13 min and 11.98 ± 0.72 min. The calibration curve was linear over the range 0.1-5.0μg/ml. The method was also suitable for the assay of paracetamol-codeine combination drug as well as estimation of the amount of constituents in urine when the wavelength of UV detection was 245 nm with acetanilide as the internal standard.