scholarly journals Robust and Sensitive High-Performance Liquid Chromatographic-UV Detection Technique for the Determination of Tigecycline in Rabbit Plasma

2011 ◽  
Vol 94 (3) ◽  
pp. 847-856 ◽  
Author(s):  
Kostas M Zorpas ◽  
Georgia N Valsami ◽  
Evangelos V Vryonis ◽  
Athanasios T Skoutelis ◽  
Helen A Archontaki
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Pharmacokinetic Profile ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmacokinetic Studies ◽  
Rabbit Plasma ◽  
Elution Time ◽  
Liquid Chromatographic

Abstract An isocratic HPLC method with detection at 248 nm was developed and fully validated for the determination of tigecycline in rabbit plasma. Minocycline was used as an internal standard. A Hypersil BDS RP-C18 column (250 × 4.6 mm, 5 μm particle size) was used with the mobile phase phosphate buffer (pH 7.10, 0.070 M)–acetonitrile (76 + 24, v/v) at a flow rate of 1.0 mL/min. The elution time of tigecycline and minocycline was approximately 8.1 and 9.9 min, respectively. Calibration curves of tigecycline were linear in the concentration range of 0.021–3.15 μg/mL in plasma. The LOD and LOQ in plasma were estimated as 7 and 21 ng/mL, respectively. The intraday and interday precision values of the method were in the range of 5.0–7.1 and 5.6–9.1%, while the corresponding accuracy values were in the ranges of 92.8–111.1 and 97.6–102.3%, respectively. At the LOQ, the intraday precision was 18.7%, while intraday and interday accuracy values were 97.3 and 98.0%, respectively. Robustness of the proposed method was studied using a Plackett-Burman experimental design. A pharmacokinetic profile is presented for confirmation of the applicability of the method to pharmacokinetic studies.

scholarly journals A New Validated RP- HPLC Method for the Determination of Nevirapine in Human Plasma

2010 ◽  
Vol 7 (3) ◽  
pp. 821-826 ◽  
Author(s):  
C. H. Venkata Kumar ◽  
D. Ananth Kumar ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Ammonium Acetate ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmacokinetic Studies ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

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.

scholarly journals Determination of Ketoconazole in tablets by using three different methods

2012 ◽  
Vol 4 ◽  
Author(s):  
Biljana Gjorgjeska
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Control Analysis ◽  
Analytical Work ◽  
Liquid Chromatographic ◽  
Hplc Analyses

Ketoconazole has been widely used as an antifungal drug  that is formulated as tablets, cream and over­the­counter ketoconazole shampoo. The aim of this research was to study and to standardize an ultraviolet spectrophotometric (UVS) method, potentiometric  and a high  performance  liquid  chromatographic  (HPLC) method  for  the determination  of ketoconazole in commercially available Oromycosal® tablets. These three methods were compared and discussed with respect to  their  sensitivity,  selectivity  and ready­applicability  in  routine  analytical  work.   Absorption  spectra and spectrophotometric determinations were carried out on the UVS spectrophotometer. Investigated concentrations were in range from  0.003 to  0.02mg?dm­3. The absorbance was measured at 224  nm.  In potentiometric  titrations  glass  and saturated (KCl) calomel electrode were used. HPLC analyses of ketoconazole were carried in the presence of econazole as internal standard. It can be concluded that the described methods are simple, fast and reliable for determination of ketoconazole in pharmaceutical preparations. The preparation of the samples is easy, the excipients do not  interfere in the methods, so they can be used in routine quality control analysis.

scholarly journals Simultaneous determination of ethinyl estradiol and drospirenone in oral contraceptive by high performance liquid chromatography

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 ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Ethinyl Estradiol ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Elution Time ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

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.

Simultaneous liquid-chromatographic determination of prednisone and prednisolone in plasma.

1988 ◽  
Vol 34 (9) ◽  
pp. 1897-1899 ◽  
Author(s):  
M H Cheng ◽  
W Y Huang ◽  
A I Lipsey
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Liquid Chromatographic Determination ◽  
Standard Solution ◽  
Liquid Chromatographic

Abstract This high-performance liquid-chromatographic (HPLC) method for simultaneous determination of prednisone and its metabolite, prednisolone, in plasma is a modification of the method of Frey et al. (Clin Chem 1979;25:1944-7). Heparinized plasma (1.0 mL) with 0.1 mL of internal standard solution (11-deoxy-17-hydroxycorticosterone, 2 mg/L) is extracted with 7.0 mL of dichloromethane, then washed sequentially with 0.1 mol/L HCl, 0.1 mol/L NaOH, and deionized water, 2.0 mL each. The extract is evaporated and the residue reconstituted with 75 microL of mobile phase, methanol/H2O (40/60 by vol). Thirty microliters of this is injected onto a reversed-phase C6 column, which is eluted at 1.4 mL/min. Analytical recoveries of prednisone and prednisolone were 94-98% and 102-106%, respectively. Day-to-day precision (CV) was 3.8% for prednisone, 6.1% for prednisolone. We encountered no interference from the 21 other steroids and 25 drugs tested. This method is simple, accurate, and precise.

scholarly journals Comparison of High-Performance Liquid Chromatographic and Microbiological Methods for Determination of Voriconazole Levels in Plasma

2000 ◽  
Vol 44 (5) ◽  
pp. 1209-1213 ◽  
Author(s):  
Sofia Perea ◽  
Gennethel J. Pennick ◽  
Asha Modak ◽  
Annette W. Fothergill ◽  
Deanna A. Sutton ◽  
...  
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmacokinetic Studies ◽  
Serum Samples ◽  
Bioassay Method ◽  
Microbiological Methods ◽  
And Control ◽  
Liquid Chromatographic

ABSTRACT A new selective high-performance liquid chromatography (HPLC) method with UV detection for the determination of the investigational triazole voriconazole in human plasma by using acetonitrile precipitation followed by reverse-phase HPLC on a C18column was compared with a simple agar well diffusion bioassay method with Candida kefyr ATCC 46764 as the assay organism. Pooled plasma was used to prepare standard and control samples for both methods. The results of analyses with spiked serum samples (run as unknowns) were concordant by the bioassay and HPLC methods, with expected values being obtained. HPLC demonstrated an improved precision (3.47 versus 12.12%) and accuracy (0.81 versus 1.28%) compared to those of the bioassay method. The range of linearity obtained by both methods (from 0.2 to 10 μg/ml for HPLC and from 0.25 to 20 μg/ml for the bioassay) includes the range of concentrations of voriconazole (from 1.2 to 4.7 μg/ml) which are considered clinically relevant. Although either methodology could be used for the monitoring of patient therapy, the smaller variability observed with HPLC compared to that observed with the bioassay favors the use of HPLC for pharmacokinetic studies.

scholarly journals Development and Validation of Ultra High Performance Liquid Chromatographic (UHPLC) Method for the Determination of Roxithromycin in the Broiler Plasma

2019 ◽  
pp. 1-8
Author(s):  
R. D. Singh ◽  
S. K. Mody ◽  
H. B. Patel ◽  
V. N. Sarvaiya ◽  
B. R. Patel ◽  
...  
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Pharmacokinetic Studies ◽  
Uv Detector ◽  
Linear Calibration ◽  
The Mean ◽  
Development And Validation ◽  
Liquid Chromatographic

Aims: The present study was designed to develop and validate the UHPLC method for quantitative determination of roxithromycin, a macrolide antimicrobial drug, in broiler plasma for the application of pharmacokinetic studies. Methodology: UHPLC apparatus comprised of ultraviolet (UV) detector was used in the present study. Chromatographic separation was performed by using reverse phase C18 column. Mobile phase was combination of buffer and 55 acetonitrile in the ratio of 55: 45. Buffer part used was 0.1% trifluoroacetic acid (v/v) having pH of 2.1. Erythromycin was used as an internal standard. Isocratic elution mode was employed with flow rate of 1 ml/min and effluents were monitored at wavelength of 220 nm. Liquid-liquid extraction using ice-cold acetonitrile was performed to extract roxithromycin from plasma samples. The data integration was performed using Chromeleon™ version 6.8 software. Results: The linear calibration curve with a mean correlation coefficient (R2) value of 0.9999 was observed for concentrations ranging from 0.20 to 12.80 µg/ml. At any concentration, accuracy was not found to be less than 90%. The mean extraction recovery (n=5) for concentrations of 0.40 µg/ml was 81.36%. The calculated intraday and interday C.V. % was not more than 7.70% and 9.42%, respectively, at any concentration studied. The specificity of the analysis was reflected by the narrow range of retention time ranging between 6.983 to 7.178 minutes. LOD and LOQ of the method under investigation were calculated as 0.131 and 0.398 µg/ml, respectively. Conclusion: A reliable, reproducible, accurate, precise, specific and sensitive method for analysis of roxithromycin in broiler plasma was developed and validated for application in the pharmacokinetic study of the roxithromycin.

High Performance Liquid Chromatographic Method for Determination of Temephos in Technical and Formulated Products: Collaborative Study

1982 ◽  
Vol 65 (3) ◽  
pp. 580-583
Author(s):  
James W Miles ◽  
Dwight L Mount
Keyword(s):  
Ethyl Acetate ◽  
High Performance ◽  
Collaborative Study ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Water Dispersible ◽  
Coefficients Of Variation ◽  
Liquid Chromatographic

Abstract An HPLC method for the determination of temephos in temephos technical and formulated products has been subjected to an international collaborative study with 14 laboratories participating. Samples were extracted with ethyl acetate and eluted on a silica gel column with ethyl acetate-hexane (1 + 9); p-nitrophenyl p-nitrobenzoate served as the internal standard. Collaborators were furnished samples of technical, 20 and 50% emulsifiable concentrates, 50% water-dispersible powder, and 1% sand granules. The coefficients of variation of the values obtained on the 5 samples were 1.21,2.02,1.26,1.89, and 9.90%, respectively. The method has been adopted official first action.

scholarly journals High-Performance Liquid Chromatographic Method for Determination of Phenytoin in Rabbits Receiving Sildenafil

2008 ◽  
Vol 3 ◽  
pp. ACI.S658 ◽  
Author(s):  
Alaa Khedr ◽  
Mohamed Moustafa ◽  
Ashraf B. Abdel-Naim ◽  
Abdulrahman Alahdal ◽  
Hisham Mosli
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Sodium Acetate Solution ◽  
Acetate Solution ◽  
Rabbit Plasma ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A validated high-performance liquid chromatographic (HPLC) method for determination of phenytoin (PHN), para-hydroxy metabolite of phenytoin (POH) and sildenafil (SIL) in rabbit plasma is described. The method is based on extraction on Sep-Pak C18 solid support using ethyl acetate and ether as eluents and monitoring at 220 nm. The extracted samples were analyzed by HPLC using Agilent Zorbax Extended C18 column (150 mm x 4.6 mm internal diameter) and isocratic elution with a mobile phase consist of 29% acetonitrile and 71% sodium acetate solution (0.02 M, pH 4.6). The method was fully validated for linearity and range, selectivity, precision, stability, recovery, and robustness. The linearity of the method was in the range of 0.15 to 39 µg /ml for PHN and 0.15 to 33 µg/ml for both POH and SIL. Limits of detection (LOD) of PHN, POH, and SIL were 0.15 ± 0.01, 0.15 ± 0.01, and 0.15 ± 0.01 µg/ml, respectively. The % recovery of PHN, POH, and SIL from rabbit plasma were, 101.88 ± 0.12, 99.16 ± 0.25, and 99.49 ± 0.33, respectively. The method was applied on plasma collected from rabbits at different time intervals after receiving 30 mg/kg PHN-Na with (and without) 8 mg/kg SIL citrate.

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