scholarly journals Determination of Ranitidine in Human Plasma by SPE and ESI-LC-MS/MS for Use in Bioequivalence Studies

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Karini B. Bellorio ◽  
Maria Isabel R. Alves ◽  
Nelson R. Antoniosi Filho

A method for determining ranitidine in human plasma by ESI-LC-MS/MS was validated, using propranolol as internal standard. The extraction method used was solid phase extraction (SPE). Chromatographic separation was performed in a Chromolith C18 (50 mm × 4.6 mm i.d.) analytical column, which provided good separation of ranitidine and propranolol peaks with an analysis time of 2.5 minutes. Extraction yields of 94.4% for ranitidine and 89.4% for the internal standard were obtained. The lower limit of quantification (LLOQ) was 3.00 ng/mL, and limit of detection (LOD) was 0.05 ng/mL, with linearity ranging from 3.00 to 500 ng/mL. The results, thus, showed that this method is suitable for application in bioequivalence studies of ranitidine in human plasma.

2010 ◽  
Vol 5 ◽  
pp. ACI.S4431 ◽  
Author(s):  
Liusheng Huang ◽  
Patricia S. Lizak ◽  
Anura L. Jayewardene ◽  
Florence Marzan ◽  
Ming-Na Tina Lee ◽  
...  

An HPLC-UV method was developed and validated for the determination of lumefantrine in human plasma. Lumefantrine and its internal standard halofantrine were extracted from plasma samples using protein precipitation with acetonitrile (0.2% perchloric acid) followed by solid-phase extraction with Hypersep C8 cartridges. Chromatographic separation was performed on a Zorbax SB-CN HPLC column (3.0 × 150 mm, 3.5 μm) with water/methanol (0.1% TFA) as the mobile phases in a gradient elution mode. Detection was performed using UV/vis detector at λ = 335 nm. The method showed to be linear over a range of 50-10,000 ng/mL with acceptable intra- and inter-day precision and accuracy. The mean recoveries were 88.2% for lumefatrine and 84.5% for the I.S. The internal standard halofantrine is readily available from commercial sources. This method was successfully applied to a pharmacokinetic interaction study between a first-line antimalarial combination (artemether—lumefantrine) and antiretroviral therapy.


2016 ◽  
Vol 35 (2) ◽  
pp. 225 ◽  
Author(s):  
Violeta Ivanova-Petropulos ◽  
Krste Tašev ◽  
Marina Stefova

<p>A solid-phase extraction method followed by reverse phase high-performance liquid chromatography (RP-HPLC) was optimized and validated for the quantitative determination of tartaric, malic, shikimic, lactic, citric and succinic acids in wine. Solid-phase extraction was carried out with C18 cartridges and extraction recoveries for all acids ranging from 98.3 to 103% were obtained. HPLC separation was performed with isocratic elution on a LiChrosorb RP-18 column (250 × 4.6 mm I.D., 5 µm) protected with the appropriate guard column. The mobile phase was a 5 mM solution of H<sub>3</sub>PO<sub>4</sub> with pH 2.1 at a flow rate of 1 ml/min. Detection of the organic acids was performed at 210 nm. The developed method was validated by checking its linearity, limit of detection (LOD), limit of quantification (LOQ), precision and recovery. The method was applied to the analysis of organic acids in Macedonian red and white wines.</p>


2005 ◽  
Vol 824 (1-2) ◽  
pp. 45-50 ◽  
Author(s):  
S RAMANATHAN ◽  
S KARUPIAH ◽  
N NAIR ◽  
P OLLIARO ◽  
V NAVARATNAM ◽  
...  

2019 ◽  
Vol 7 (11) ◽  
pp. 1757-1761 ◽  
Author(s):  
Dragica Zendelovska ◽  
Emilija Atanasovska ◽  
Kalina Gjorgjievska ◽  
Kristina Pavlovska ◽  
Krume Jakjovski ◽  
...  

BACKGROUND: A new simple, selective and accurate high-performance liquid chromatographic (HPLC) method utilising solid-phase extraction for the determination of pantoprazole in human plasma samples has been developed. AIM: The purpose of this paper was developing a new HPLC method suitable for the determination of pantoprazole in plasma samples, which enables simple and rapid isolation and concentration of the analysed drug.METHODS: The chromatographic separation was accomplished on a LiChroCart LiChrospher 60 RP select B column using a mobile phase composed of 0.2 % (V/V) water solution of triethylamine (pH 7) and acetonitrile (58:42, V/V) followed by UV detection was at 280 nm. The solid-phase extraction method using LiChrolut RP-18 (200 mg, 3 ml) was applied to the obtained good separation of investigated drug from endogenous plasma components. Best results were achieved when plasma samples were buffered with 0.1 mol/L KH2PO4 (pH 9) before extraction, eluted and reconstituted with acetonitrile and 0.001 mol/L NaOH after extraction, respectively. RESULTS: The standard calibration curves showed good linearity within the range of 25.0-4000.0 ng/mL with a correlation coefficient greater than 0.996. Retention times of pantoprazole and internal standard, lansoprazole was 4.1 and 6.0 min respectively. The limit of quantification was 25.0 ng/mL. For intra- and inter-day precision relative standard deviations ranged from 4.2 to 9.3%. The relative errors for stability investigations were ranged from 0.12 to -10.5%. CONCLUSION: This method has good precision and accuracy and was successfully applied to the pharmacokinetic and bioequivalence study of 40 mg pantoprazole in healthy volunteers.


2012 ◽  
Vol 1 (11) ◽  
pp. 342-352 ◽  
Author(s):  
Mokkaisamy Jegadeesh Raja ◽  
Jegadeesh Raja Kavitha ◽  
Kothamasu Pavan Kumar ◽  
Thangavel Sivakumar

A simple, rapid, specific, sensitive and liquid chromatography coupled with tandem mass spectrophotometric method was developed and validated for the estimation of azathioprine and its metabolite 6-mercaptopurine in human plasma by using lamivudine and 6-mercaptopurine D3 as the internal standard. Azathioprine and 6-mercaptopurine were extracted from human plasma by solid-phase extraction (SPE)-Evaporation method, using Oasis MCX cartridge for cleaning procedure. The stationary phase was chromatographed on a ZORBAX SB CN, (75X50 mm, 5 µ) column where as mobile phase constitutes of acetonitrile: 2mM ammonium acetate (70:30 v/v) at a flow rate of 0.800 ml/min. The detection was performed with an Applied Biosystems Sciex API 4000 mass spectrometer by multiple reaction monitoring (MRM). The method validation proofs were carried out as per the USFDA guidelines as described, showing a linearity system (r2 > 0.99) over a range of 2.455 ng/mL to 106.568 ng/mL for azathioprine and 1.165 ng/mL to 101.143 ng/mL concentrations for 6-mercaptopurine and a recovery shows 99.36% and 100.44% for azathioprine and 6-mercaptopurine respectively. The results show that this proposed approach is effective and can be applied to the extraction and analysis of other pharmaceutical compounds.DOI: http://dx.doi.org/10.3329/icpj.v1i11.12059 International Current Pharmaceutical Journal 2012, 1(11): 342-352 


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