Development and Application of HPLC Method for Clinical Pharmacokinetic Study of Domperidone

Author(s):  
Prasad Neerati ◽  
Bhargavi Latha A ◽  
Y. Shravan Kumar ◽  
Y Madhusudan Rao

A simple and sensitive high performance liquid chromatographic method for quantification of domperidone in human serum was developed and validated. Domperi-done and internal standard (IS) propranolol hydrochloride were extracted into acetonitrile and separated using an isocratic mobile phase on a Phenomenx C18 column. The eluent was monitored by UV detector at 270 nm at a flow rate of 1.0 mL min–1. The linearity range of proposed  method was 2.5–1000 ng/ml. The intra-day and inter-day coefficient of variation and percent error values of the assay method were less than 15% and mean recovery was more than 97 and 96% for domperidone and IS, respectively. The method was found to be precise, accurate and specific during the study. The method was successfully applied for pharmacokinetic study of domperidone in humans.  

2008 ◽  
Vol 5 (s2) ◽  
pp. 1149-1153 ◽  
Author(s):  
A. Lakshmana Rao ◽  
B. N. V. Ravi Kumar ◽  
G. G. Sankar

A simple, rapid, sensitive and precise High Performance Liquid Chromatographic (HPLC) method has been developed for the estimation of rabeprazole in bulk and tablet dosage form. In this method RP-C18column (150 mm x 4.6 mm I.D, 5 µ m particle size) with mobile phase consisting of methanol and water in the ratio of 65:35 v/v in isocratic mode was used. The detection wavelength is 284 nm and the flow rate is 0.8 mL/min. Tinidazole is used as internal standard. In the range of 0.25-20 µ g/mL, the linearity of rabeprazole shows a correlation coefficient of 0.9999. The drug and internal standard were eluted at 4.41± 0.05 and 2.16± 0.04 min. respectively. The intra- and inter-day variation was found to be less than 1% showing high precision of the assay method. The detection limit was found to be 100 ng/mL. The mobile phase selected for the proposed method is simple, fast, accurate and precise and hence can be applied for routine quality control analysis of rabeprazole in bluk and its tablet dosage from.


2017 ◽  
Vol 1 (2) ◽  
pp. 1-8
Author(s):  
Milena Cristina Ribeiro Souza Magalhães ◽  
Alisson Samuel Portes Caldeira ◽  
Hanna De Sousa Rocha Almeida ◽  
Sílvia Ligório Fialho ◽  
Armando Da Silva Cunha Junior

A reversed-phase high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of encapsulation efficiency of zidovudine in nanoparticules. The method was carried out in isocratic mode using 0.040M sodium acetate: methanol: acetonitrile: glacial acetic acid (880:100:20:2) as mobile phase, a C8 column at 25ºC and UV detection at 240 nm. The method was linear (r2 ˃ 0.99) over the range of 25.0-150.0 μg/mL, precise (RSD ˂ 5%), accurate (recovery = 100.5%), robust and selective. The validated HPLC-UV method can be successfully applied to determine the rate of zidovudine in nanoparticules.


2009 ◽  
Vol 92 (5) ◽  
pp. 1602-1606 ◽  
Author(s):  
María A Rosasco ◽  
Rita Ceresole ◽  
Clara C Forastieri ◽  
Adriana I Segall

Abstract An isocratic HPLC method was developed and validated for the quantitation of methocarbamol in the presence of its degradation products. Quantitation was achieved using a reversed-phase C18 column at ambient temperature with mobile phase consisting of methanolwatertetrahydrofuran (25 + 65 + 10, v/v). The flow rate was 0.9 mL/min. The detection was by UV light at 274 nm. The proposed method was validated for selectivity, precision, linearity, and accuracy. The assay method was found to be linear from 159.0 to 793.2 g/mL (3.2 to 15.9 g injected). All validation parameters were within the acceptable range. The developed method was successfully applied to estimate the amount of methocarbamol in a veterinary injection.


2013 ◽  
Vol 49 (3) ◽  
pp. 521-528 ◽  
Author(s):  
Viviane Benevenuti Silva ◽  
Angel Arturo Gaona Galdos ◽  
Cintia Maria Alves Mothe ◽  
Michele Bacchi Pallastrelli ◽  
Maria Segunda Aurora Prado ◽  
...  

A simple, rapid, economical and reliable high performance liquid chromatographic method has been developed and successfully applied in simultaneous determination of ethinyl estradiol and drospirenone in coated tablets. The HPLC method was performed on a LiChroCART® 100RP column (125x4 mm i.d., 5 µm) with acetonitrile:water 50:50 (v/v) as mobile phase, pumped at a flow rate of 1.0 mL.min-1. The fluorescence detection for ethinyl estradiol was made at λex= 280 nm and λem= 310 nm and a UV detection for drospirenone was made at 200 nm. The elution time for ethinyl estradiol and drospirenone were 4.0 and 5.7 min, respectively. The method was validated in accordance to USP 34 guidelines. The proposed HPLC method presented advantages over reported methods and is suitable for quality control assays of ethinyl estradiol and drospirenone in coated tablets.


2008 ◽  
Vol 73 (6) ◽  
pp. 665-671 ◽  
Author(s):  
Snezana Mitic ◽  
Gordana Miletic ◽  
Danijela Kostic ◽  
Daniela Naskovic-Ðokic ◽  
Biljana Arsic ◽  
...  

An accurate, sensitive and reproducible high performance liquid chromatographic (HPLC) method for the quantification of doxycycline hyclate in pharmaceutical samples has been developed and validated. The drug and the standard were eluted from a Lichrosorb RP-8 (250 mm x 4.6 mm, 10 mm particle size) at 20?C with a mobile phase consisting of methanol, acetonitrile and 0.010 M aqueous solution of oxalic acid (2:3:5, v/v/v). The flow rate was 1.25 ml min-1. A UV detector set at 350 nm was used to monitor the effluent. Each analysis required no longer than 4 min. The limits of detection and quantification were 1.15 and 3.84 ?g ml-1, respectively. Recoveries for different concentrations ranged from 99.58 to 101.93%.


Pharmacia ◽  
2019 ◽  
Vol 66 (1) ◽  
pp. 1-5 ◽  
Author(s):  
Lily Peikova ◽  
Diana Tzankova ◽  
Alexandrina Dineva ◽  
Maya Georgieva ◽  
Alexander Zlatkov

A reversed phase enantio selective high performance liquid chromatographic method was developed for enantiomeric separation of 2-(1,3-dimethyl-2,6-dioxo-2,3-dihydro-1H-purine-7(6H)-yl)-N'-(3-fluorobenzylidene)-propanehydrazide isomers. The enantiomers of 2-(1,3-dimethyl-2,6-dioxo-2,3-dihydro-1H-purine-7(6H)-yl)-N'-(3-fluorobenzylidene)propanehydra-zide were resolved on a ACEÒEquivalenceTM С18 (250 × 4.6 mm, 5 μm) column using a mobile phase system containing methanol, water, phosphate buffer рН 7.4 (50:46:4 v/v/v). The resolution between enantiomers was found to be more than 2.0. The sample solution and mobile phase were found to be stable for at least 48 h. The final optimized method was successfully applied to separate the (R)- and the (S)-enantiomers of 2-(1,3-dimethyl-2,6-dioxo-2,3-dihydro-1H-purine-7(6H)-yl)-N'-(3-fluorobenzylidene)-propanehydrazide and was proven to be reproducible and accurate.


2010 ◽  
Vol 7 (3) ◽  
pp. 821-826 ◽  
Author(s):  
C. H. Venkata Kumar ◽  
D. Ananth Kumar ◽  
J. V. L. N. Seshagiri Rao

A rapid, selective and sensitive high performance liquid chromatographic method for the estimation of nevirapine in human plasma has been developed. Chromatography was carried out on a Hypersil BDS C18column using a mixture of ammonium acetate buffer (pH 4.0 ± 0.05) and acetonitrile (85:15 v/v) as the mobile phase. The eluents were monitored for the drug by UV detection at 254 nm. Oxcarbazepine was used as an internal standard for this study. The retention times for nevirapine and oxcarbazepine were found to be 7.2 and 14.7 min respectively. The method was found to be linear in the concentration range of 50 ng/mL to 5003.7 ng/mL. The method was validated as per FDA guidelines and was found to be suitable for bioequivalence and pharmacokinetic studies.


1980 ◽  
Vol 63 (6) ◽  
pp. 1291-1295
Author(s):  
Mikio Chiba ◽  
D F Veres

Abstract A simple HPLC method has been developed to individually determine residues of benomyl and MBC on apple leaves without cleanup. Sample leaves in a Mason jar are freeze-dried and tumbled for extraction in CHC13 containing 5000 μg n-propyl isocyanate/mL at 1°C. n-Butyl isocyanate is added to the extract at 5000 μg/mL, and 20 μL of the mixture is injected into the HPLC system. A Brownlee LiChrosorb silica gel column with a guard column is operated with a mixed mobile phase of chloroform-hexane (4+1) saturated with water. MBC, present as a degradation compound of benomyl, is identified as methyl 1 – (n – propylcarbamoyl) – 2 – benzimidazole carbamate (MBC-n-PIC derivative). At 280 nm, both benomyl and MBC-n-PIC can be detected with a UV detector at a level of 0.2 ppm in apple leaves.


2011 ◽  
Vol 47 (2) ◽  
pp. 261-268 ◽  
Author(s):  
Elisabete de Almeida Barbosa Antunes ◽  
Felipe Rebello Lourenço ◽  
Terezinha de Jesus Andreoli Pinto

A high-performance liquid chromatographic method employing pre-column derivatization with o-phthalaldehyde (OPA) and 2-mercaptoacetic acid was developed for the determination of apramycin, an aminoglycoside antibiotic used in veterinary medicine, in the oral soluble powder form. The chromatographic separation was done by ion-pair HPLC using a C18 reversed-phase column, Synergy Hydro (150 mm x 4.6 mm x 4 µm) and mobile phase composed of 0.005 mol/L sodium octanosulfonate in a mixture of acetonitrile: water: acetic acid (45:55:2) (v/v/v) with a flow rate of 1.0 mL/min; the UV detector was operated at 332 nm. The developed method was validated according to official compendia guidelines, having demonstrated robustness, selectivity and linearity for the concentration range of 0.02 to 0.05 mg/mL, precision (with RSD < 2.0% both for intra and inter-day precision) accuracy (average recuperation of 99.33%) and detectivity (quantification and detection limits of 0.08 and 0.02 µg/mL, respectively). Three batches of commercial apramycin oral soluble powder were analyzed by both the proposed method and the official microbiological method, where all the results obtained were in the acceptable range (95% to 105% of labeled value of apramycin). Both methods were statistically compared by the t test, which yielded no significant differences (α = 0.05) thereby confirming the equivalence of the methods.


1983 ◽  
Vol 29 (5) ◽  
pp. 851-853 ◽  
Author(s):  
T Okuda ◽  
T Oie ◽  
M Nishida

Abstract We describe the adaptation of a "high-performance" liquid chromatographic method for determination of creatinine in serum and urine. The proposed method is simple, rapid, precise, and accurate. The retention time for creatinine can be varied simply by changing the KH2PO4 concentration in the mobile phase: acetonitrile/aqueous KH2PO4 (1/4 by vol). Within-day precision (CV) was 1.2-3.6% in serum chromatographed with an internal standard, and 2.3-2.8% in serum when an external standard was used. Between-day precision (CV) was 1.3-2.1% in serum and 1.3-2.7% in urine (with an external standard). Analytical recoveries of creatinine added to serum were 94-100% for the method with an internal standard, 95-103% with an external standard.


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