Determination of Ibuprofen in human plasma with minimal sample pretreatment (original) (raw)
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WORLD JOURNAL OF PHARMACY AND PHARMACEUTICAL SCIENCES
A simple, precise, and rapid reversed-phase high performance liquid chromatography (HPLC) method for the determination of ibuprofen (IBU) in human plasma using gemfibrozil as an internal standard (IS) was developed and validated. Plasma samples containing ibuprofen were spiked with the IS, precipitated with methanol, and centrifuged. The compounds of interest were efficiently separated on Symmetry Shield RP18 column maintained at a temperature of 40C, and detected with multi-wave length fluorescence detector (excitation/emission wavelength 230/ 275 nm). The mobile phase consisted of 0.01M dibasic ammonium phosphate (pH adjusted to 5.5 with phosphoric acid) and acetonitrile (45:55, v:v), and was delivered at a flow rate of 1.5 ml/min. The relationship between ibuprofen concentration in plasma and peak area ratio of ibuprofen / IS was linear (R2 0.9997) in the range of 0.25 -60 μg/ml, the intraand inter-day coefficient of variations (CV) were ≤ 3.8% and ≤ 2.9%, respectively. Extraction recoveries of ibuprofen and the IS were > 90%, whereas the accuracy (relative recovery) of ibuprofen measurement was 98% to 107% using quality control samples and 92% to 105% as determined by back calculation from peak area ratios of the calibration curves. The method was used to assess the stability of ibuprofen in human plasma under various conditions in the clinical laboratory. Further, it was successfully employed to measure ibuprofen levels in samples obtained normal volunteer. W WO OR RL LD D J JO OU UR RN NA AL L O OF F P PH HA AR RM MA AC CY Y A AN ND D P PH HA AR RM MA AC CE EU UT TI IC CA AL L S SC CI IE EN NC CE ES S S SJ JI IF F I Im mp pa ac ct t F Fa ac ct to or r 2 2. .7 78 86 6
RP-HPLC ASSAY OF IBUPROFEN IN PLASMA USING DIFFERENT EXTRACTION PROCEDURES
An isocratic reverse phase high performance liquid chromatographic (RP-HPLC) method with ultra violet detection at 220 nm was used for a simple, selective and precise quantitation of a non-steroidal anti-inflammatory drug i.e. ibuprofen (IBF) from rat plasma. The procedure employed mefenamic acid as an internal standard (IS). A good chromatographic separation between IBF, the internal standard and interfering endogenous peaks was achieved using a Octadecyl Silane column and acetonitrile (ACN)-water-methanol-ortho phosphoric acid (in ratio of 58: 37: 5: 0.05 v/v/v/v) as the mobile phase at a flow rate of 1.0 ml/min. Two extraction procedures for RP-HPLC quantitation of IBF were analysed. In the first method acetonitrile was used for extraction of the drug from plasma whereas the second method involved extraction of drug from plasma using diethyl ether. The second method proved to be more suitable for quantitation of the drug from plasma. The applicability of procedure includes the requirement of less sample volume, lesser organic solvent consumption and good plasma clean up for pharmacokinetic studies, in case of small animals, neonates and children as well.
Determination of Ibuprofen in Human Plasma and Urine by Gas Chromatography/Mass Spectrometry
Journal of AOAC INTERNATIONAL, 2014
This paper describes a GC/MS method for the determination of ibuprofen in human plasma and urine. Ibuprofen and internal standard naproxen were extractedfrom plasma and urine by using a liquid–liquid extraction method. Derivatization was carried outusing N-methyl-N-(trimethylsilyl) trifluoroacetamide. Calibration curves were linear over the concentration range of 0.05–5.0 and 0.1–10.0 μg/mL for plasma and urine, respectively. Intraday and interday precision (RSD) values for ibuprofen in plasma and urine were less than 6.31%, and accuracy (relative error) was better than 12.00%. The mean recovery of ibuprofen was 89.53% for plasma and 93.73% for urine. TheLOD was 0.015 and 0.03 μg/mL and the LOQ was 0.05 and 0.1 μg/mL for plasma and urine, respectively. The method was successfully applied to blood samples from three healthy male volunteers who had been given an oral tablet of 600 mg ibuprofen.
Journal of chromatography, 1988
A sensitive and selective high-performance liquid chromatographic assay for free and total ibuprofen and its major metabolites in human urine is described. Urine is acidified, drug and metabolites are extracted into hexane-propanol, back-extracted into sodium bicarbonate, neutralized and chromatographed. Ibufenac (4-isobutylphenylacetic acid) and 2-phenylpropionic acid were employed as internal standards. The extraction efficiencies were 94-100% for all compounds. The two metabolites and their internal standard were separated using an isocratic chromatographic system, followed by an abrupt step gradient to a second eluent for separation of ibuprofen and its internal standard with a total run time of 18 min. Detection was by a fixed-wavelength detector (214 nm). Sample-to-sample and day-to-day reproducibility studies yielded coefficients of variability of less than 9% for all compounds. The sensitivity was sufficient to determine 2.5 micrograms/ml free ibuprofen in 100 microliters ur...
Asian Journal of Pharmaceutics, 2019
Context: In this manuscript, high-performance liquid chromatography technology equipped with ultraviolet detector has been developed that it has the sensitivity, accuracy, and high reliability for the simultaneous identification of the ibuprofen (IB) and paracetamol (PA). Methods: Chromatographic separation was achieved on Ion Pac column; Arcus EP-C18 (5 μm, 4.6 mm × 250 mm) by a mobile phase consisted of acetonitrile and water (30:70, v/v)+40 mmol/L phosphate buffer at pH 6.0 with a flow rate of 1.0 mL/min. The detection wavelength was set range at 300–330 nm. The IB and PA were subjected to different forced degradation conditions. In all the conditions, the degradation products were well obtained from the peaks of IB and PA. The method was linear at a concentration range of 5–25 μg/mL (R2 = 0.9987) and 1–5 μg/mL (R2 = 0.9989) for the IB and PA, respectively. Results: The limit of detection (LLOD) was 0.0133 μg/mL and limit of quantitation (LLOQ) was 0.0420 μg/mL for IB and the LLO...
Identification and Quantification of Ibuprofen in Blood Using HPLC-UV/Vis
2017
approved:_________________________________________ Non-steroidal anti-inflammatory drugs are some of the most frequently used medications in the United States. Ibuprofen is a common over-the-counter nonnarcotic analgesic, and it is also typically used as an antipyretic and as an anti-inflammatory. Intentional or unintentional ibuprofen overdose is common but typically found to be non-life threatening. If a victim had decreased hepatic or renal function, however, ibuprofen overdoses may impart significant toxicity, and at high dosages, it has been linked to cardiovascular events. Currently, the Sedgwick County Regional Forensic Science Center (RFSC) sends postmortem samples to a contract laboratory if ibuprofen toxicity is suspected. The purpose of this project is to develop and validate a method for the detection and quantitation of ibuprofen for RFSC using High Performance Liquid Chromatography (HPLC) with a UV/Vis detector. Ibuprofen and an internal standard, otoluic acid were added to negative blood and extracted using acetate buffer (pH 4.5) and ethyl acetate/ hexane 50/50 over a range of concentrations (40 mg/L-450 mg/L). Using the Breeze 2 software package, a calibration curve was generated and various test concentrations were quantitated. The method was validated in accordance with the Scientific Working Group for Forensic Toxicology (SWGTOX) guidelines. Actual concentrations (as measured by the Breeze 2 software) were within ±20% of the expected concentrations. This method is a cost-effective option for rapid ibuprofen analysis.
A simple and fast isocratic Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method has been developed and validated for the simultaneous determination of Paracetamol and Ibuprofen in tablets. The method consists of a mobile phase combination of Methanol (HPLC grade) and 0.025 M phosphate buffer adjusted to pH 3.0 with orthophosphoric acid in the ratio 80:20 using Eurospher 100-5 C18 (250 x 4.6) mm (Knauer Column with precolumn) as the stationary phase. The flow rate was 1.0 mL/min at ambient temperature conditions. With Caffeine as the internal standard, quantification was achieved with UV detection at 225 nm. A good resolution and a short run time of 12 minutes were achieved with the validated conditions. The retention times of Paracetamol, Ibuprofen and Caffeine were 2.864±0.005, 4.011±0.006 and 7.678±0.007 respectively. The method was found to be specific, robust, accurate and precise for the estimation of Paracetamol and Ibuprofen in Paracetamol and Ibuprofen fixed dose tablets over the concentration ranges of 0.00584 % w/v-0.00876 % w/v and 0.00709 % w/v-0.001063 % w/v respectively. The Correlation Coefficient (r 2) for Paracetamol and Ibuprofen were greater than 0.999. The purpose of this study was to develop and validate a simple HPLC method for the estimation of Paracetamol and Ibuprofen in combined dosage forms. The proposed method is precise, specific, accurate and robust for the simultaneous estimation of Paracetamol and Ibuprofen in dosage forms.