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RP-HPLC–UV method for the quantification of propranolol in rat's serum and krebs buffer using one-step protein precipitation

Al Shaker H., Qinna Nidal A., Hroub H., Omari M. M. H., Adnan A.

Acta Chromatographica

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2018

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Vol. 30, no. 3

147--152

EN

Krebs buffer is considered one of the most used physiological buffers in biomedical research. In the current work, a rapid reversed-phase high-performance liquid chromatographic (RP-HPLC) method with ultraviolet (UV) detection at 214 nm was developed and validated according to European Medicines Evaluation Agency (EMEA) guidelines for the determination and quantification of propranolol in Sprague–Dawley rat's serum and in Krebs buffer. This method can be applied for both in vivo and in vitro studies with short run time of 7.0 min . Isocratic elution with a flow rate of 1.0 mL/min was employed. BDS Hypersil C-18 column (150 mm × 4.6 mm and 5 μm) was used to obtain satisfactory resolution. The mobile phase used contained a mixture of acetonitrile, methanol, and triethylammonium phosphate solution (15.0:32.5:52.5, v/v). Best separation between propranolol and the internal standard (I. S.) sildenafil was obtained at 4.2 and 5.5 min, respectively. Propranolol was linear over a concentration range of 50.00–3000 ng/mL with acceptable accuracy, and intra- and inter-day precision. Dilution integrity was assessed and was found to be within the acceptable range for both serum and Krebs buffer. Sample stability tests were studied at different storage conditions, and all the analytes were found to be stable. The mean percentage of recovery of propranolol was found to be 97.06% and 98.57% for serum and Krebs buffer, respective.

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Isolation of gallic acid and methyl gallate from folium Toonea Sinensis and validated method for their quantitation using LC-based technologies

Shen Y., Yang H., Xia G., Wang J., Cai B., Jia X.

Acta Chromatographica

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2013

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Vol. 25, no. 4

687--701

EN

Silica-gel column chromatography and preparative reversed-phase high-performance liquid chromatography (RP-HPLC) were sequentially employed for the isolation of two antioxidants including gallic acid and methyl gallate from Folium Toonea Sinensis. An RP-HPLC-UV method was then developed and validated to rapidly determine their content in this herb with ethyl gallate as internal standard. The quantitation was performed on an XBridge Shield RP18 column (150 mm × 4.6 mm, 5 μm) under 40°C. The mobile phase consisting of acetonitrile and 0.1% formic acid aqueous solution was driven at 1.0 mL min -1 under gradient elution, and 270 nm was selected to monitor the separation. To evaluate the fitness for purpose of the method and to investigate the difference in the content of analytes among different samples, the leaves collected from five production sites were analyzed. The newly established method is suitable for routine analysis of gallic acid and methyl gallate in the herb and, hence, can assist in its quality assessment. It was also found that not only the content of two antioxidants but also the ratio varied significantly among different geographical origins. In addition, three samples from Yantai, Zumadian, and Zhenjiang were distinguished as they have a much higher content ratio than the other two.

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Development and validation of an RP-HPLC-UV method for the determination of ondansetron in rabbit plasma: Application to a pharmacokinetic study

Ravi S., Khan N., Darwis Y

Acta Chromatographica

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2011

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Vol. 23, no. 4

579--593

EN

A new sensitive and specific isocratic RP-HPLC-UV method was developed and validated for the determination of ondansetron in rabbit plasma using risperidone as an internal standard (IS). The sample preparation involved a simple deprotenization procedure with a mixture of 1 mL of acetonitrile and 50 μL of 10% w/υ zinc sulfate. Analysis was performed on a Phenomenex CN column (250 mm × 4.6 mm, 5 μm) with 50 mM ammonium acetate (pH 3.5) and acetonitrile (35:65, υ/υ) as mobile phase at a flow rate of 1.0 mL min-1. Column eluent was monitored at 310 nm. The calibration curve was linear over the concentration range of 25–1000 ng mL-1. (r2 = 0.9999) with a limit of quantification (LOQ) 25 ng mL. -1.The intraday and interday precision and accuracy were between 0.93% and 3.41% and −3.63% and 1.01%, respectively. The mean recoveries of ondansetron and risperidone were 85.87% and 99.80%, respectively. Ondansetroncontaining plasma samples were stable at −20°C for 14 days. The validated method was successfully applied for a pharmacokinetic study after a single oral administration of ondansetron (8 mg) to rabbits.

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Development and validation of an RP-HPLC-UV method for analysis of sumatriptan succinate in pharmaceutical dosage forms

Ravi S., Darwis Y, Khan N

Acta Chromatographica

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2009

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Vol. 21, no. 3

421--432

EN

An isocratic RP-HPLC-UV method for analysis of sumatriptan succinate in pharmaceutical dosage forms has been developed and validated. Best separation was achieved on a Thermo Hypersil C4 column (250 mm × 4.6 mm, 5 µm) using a mobile phase of 20 mM potassium dihydrogen phosphate adjusted to pH 4.0 with orthophosphoric acid and acetonitrile (65:35, v/v) at a flow rate of 1.0 mL min -1. UV detection was performed at 227 nm. The method was validated for specificity, linearity, precision, accuracy, limit of quantification, limit of detection, robustness, and solution stability. The calibration plot was linear over the concentration range 25–600 ng mL -1 (r 2= 0.9998) and the limits of detection and quantification were 10 and 25 ng mL -1, respectively. Intra-day and inter-day precision and accuracy were between 1.25 and 2.95% and between −1.15 and 2.47%, respectively. The method was successfully used for analysis of sumatriptan succinate, in the presence of excipients, in orally disintegrating tablets prepared in our laboratory and in commercially available tablets (Imigran) and nasal spray (Suminat).