scholarly journals Comparative evaluation of moxifloxacin MDR-TB drug; as microspheres with respect to pure drug in lung tissue

2016 ◽  
Vol 2 (2) ◽  
pp. 103
Author(s):  
Sanaul Mustafa ◽  
V.Kusum Devi
Keyword(s):  
Oral Administration ◽  
Lung Tissue ◽  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Uv Detector ◽  
Relative Standard ◽  
Emulsification Solvent Evaporation

A novel moxifloxacin (MOX)-loaded poly (DL-lactide-co-glycolide) (PLGA) microspheres (MPs) suitable for oral administration was prepared by double emulsification solvent evaporation (w/o/w) method. To investigate the pharmacokinetic of MOX-MPs, a simple and rapid high performance liquid chromatographic method was developed for the quantification of MOX in plasma and lung tissue of rats treated with MOX-MPs. Gatifloxacin (0.2µg/ml) was used as an internal standard (IS). The chromatographic separation was achieved on a reversed phase C18 column using isocratic elution with (0.01% Triethanolamine in distilled water): Acetonitrile in the ratio 70:30 v/v pH 2 adjusted with ortho-phosphoric acid, at flow rate of 1 ml/min with a total run time of 6 min. The column effluent was monitored by UV detector at 290 nm. The assay was found to be linear and validated over the concentration range 0.025 to 3.2 µg/ml for MOX in plasma and 0.1 to 2.5 µg/g of lung tissue with correlation coefficient of r2 0.9998 and r2 0.9997 respectively. The system was found to construct sharp peaks for MOX and IS with retention times of 4.08 (±0.012) and 5.84 (±0.026) min for plasma, and 4.17 (±0.016) and 5.84 (±0.022) for lung tissue, respectively. The method exhibited accuracy, precision (inter-day relative standard deviation (RSD) and intra-day RSD values < 15.0 %. The method was applied for determining MOX concentration in plasma and lung after oral administration of 10mg/kg of free MOX and MOX MPs to rats. Results established selectivity and suitability of the method for pharmacokinetic studies of MOX from MOX-MPs

scholarly journals Simple and Rapid Liquid Chromatography Method for Determination of Rifabutin in Plasma

2013 ◽  
Vol 9 (2) ◽  
pp. 26-29 ◽  
Author(s):  
AK Hemanth Kumar ◽  
V Sudha ◽  
Geetha Ramachandran
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Chromatography Method ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

A high performance liquid chromatographic method for determination of rifabutin in human plasma was  developed. The method involved deproteinisation of the sample with acetonitrile and analysis of the  supernatant using a reversed-phase C18 column (250mm) and UV detection at a wavelength of 265nm.  The assay was specific for rifabutin and linear from 0.025 to 10.0μg/ml. The relative standard deviation  of intra- and inter-day assays was lower than 10%. The method was able to remove interfering materials  in plasma, yielding an average recovery of rifabutin from plasma of 101%. Due to its simplicity, the assay  can be used for pharmacokinetic studies of rifabutin. SAARC Journal of Tuberculosis, Lung Diseases & HIV/AIDS; 2012; IX(2) 26-29 DOI: http://dx.doi.org/10.3126/saarctb.v9i2.7975

scholarly journals Nonextractive Procedure and Precolumn Derivatization with 7-Chloro-4-nitrobenzo-2-oxa-1,3-diazole for Trace Determination of Trimetazidine in Plasma by High-Performance Liquid Chromatography with Fluorescence Detection

2008 ◽  
Vol 91 (5) ◽  
pp. 1037-1044 ◽  
Author(s):  
Ibrahim A Darwish ◽  
Ashraf M Mahmoud ◽  
Nasr Y Khalil
Keyword(s):  
Human Plasma ◽  
Fluorescence Detection ◽  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Pharmacokinetic Studies ◽  
Precolumn Derivatization ◽  
Trace Determination ◽  
Relative Standard

Abstract A highly sensitive high-performance liquid chromatographic method with fluorescence detection has been developed and validated in a single laboratory for the trace determination of trimetazidine (TMZ) in human plasma. Fluoxetine (FLX) was used as the internal standard. TMZ and FLX were isolated from plasma by protein precipitation with acetonitrile and derivatized by heating with 7-chloro-4-nitrobenzo-2-oxa-1,3-diazole in pH 8 borate buffer at 70C for 30 min. Separations were performed in the isocratic mode on a Nucleosil CN column with the mobile phase acetonitrile10 mM sodium acetate buffer (pH 3.5)methanol (47 + 47 + 6, v/v/v) at a flow rate of 1.0 mL/min. The derivatized samples were excited at 470 nm and monitored at an emission wavelength of 530 nm. Under the optimum chromatographic conditions, a linear relationship with a good correlation coefficient (r 0.9997, n 5) was obtained for the peak area ratio of TMZ to FLX and for TMZ concentrations of 1120 ng/mL. The proposed method has the lowest limits of detection and quantitation reported to date for the determination of TMZ in plasma with values of 0.3 and 0.95 ng/mL, respectively. The values for intra- and interassay precision were satisfactory; the relative standard deviations were 4.04. The accuracy of the method was demonstrated; the recoveries of TMZ from spiked human plasma were 98.13102.83 0.24.04. The method has high throughput because of its simple sample preparation procedure and short run time (&lt;10 min). The results demonstrated that the proposed method would have great value when applied in pharmacokinetic studies for TMZ.

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.

scholarly journals DETERMINATION OF 5H-BENZO[2,3][1,4]OXAZEPINO[5,6-B]INDOLES IN RAT PLASMA BY REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC-ULTRAVIOLET METHOD: APPLICATION TO PHARMACOKINETIC STUDIES

2017 ◽  
Vol 10 (12) ◽  
pp. 425 ◽  
Author(s):  
Ashok K Singh ◽  
Vinit Raj ◽  
Amit Rai ◽  
Amit K Keshari ◽  
Pranesh Kumar ◽  
...  
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Rat Plasma ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Relative Standard ◽  
Liquid Chromatographic

Objective: Recently, we reported newly synthesized 5H-benzo[2,3][1,4]oxazepino[5,6-b]indole) derivatives and proved their cytotoxicity against hepatocellular carcinoma specific Hep-G2 cell lines. We attempted herein to describe a reversed-phase high-performance liquid chromatographic method for the determination of three most active compounds 6a, 10a, and 15a in rat plasma to predict their pharmacokinetics parameters before in vivo study.Methods: A rapid and sensitive reversed-phase high-performance liquid chromatographic was employed for the determination of 6a, 10a, and 15a in rat plasma. Each compound was separated by a gradient elution of acetonitrile and water with 1 mL/min flow rate. The detector was set at 270, 285, and 275 nm for 6a, 10a, and 15a and the recorded elution times were 2.00, 2.87, and 1.88 min, respectively.Results: The calibration curve was linear with R2 of 0.938, 0.875, and 0.923 over the concentration range of 0.1–50 μg/mL. The inter- and intra-day variations of the assay were lower than 12.26%; the average recovery of 6a, 10a, and 15a was 97.31, 92.56, and 95.23 % with relative standard deviation of 2.12%, 3.25%, and 2.28%, respectively. The Cmax and Tmax were ~ 46.34, 18.56, and 25.65 μg/mL and 2.0, 4.0, and 4.0 h for 6a, 10a, and 15a, respectively, which indicate a robust method of detection in the present experiment.Conclusion: The study suggests that all of the three compounds have a lower rate of absorption, higher volume of distribution, and lower clearance rate, indicating good therapeutic response for in vivo activity. 

scholarly journals Determination of donepezil hydrochloride in human plasma and pharmaceutical formulations by HPLC with fluorescence detection

2011 ◽  
Vol 61 (4) ◽  
pp. 403-413 ◽  
Author(s):  
Mohammed Abonassif ◽  
Mohammed Hefnawy ◽  
Mohamed Kassem ◽  
Gamal Mostafa
Keyword(s):  
Human Plasma ◽  
Fluorescence Detection ◽  
High Performance ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Relative Standard ◽  
Donepezil Hydrochloride

Determination of donepezil hydrochloride in human plasma and pharmaceutical formulations by HPLC with fluorescence detectionA sensitive, isocratic reversed-phase high performance liquid chromatographic method involving fluorescence detection was developed for the determination of donepezil hydrochloride in tablets and in human plasma. Pindolol was used as an internal standard. Good chromatographic separation was achieved by using an analytical column C18. The system operated at room temperature using a mobile phase consisting of methanol, phosphate buffer (0.02 mol L-1) and triethyl amine (pH 3.5) (55: 45: 0.5,V/V/V) at a flow rate 0.9 mL-1min. The analyte and internal standard were extracted from human plasmavialiquid-liquid extraction. The proposed method was validated for sensitivity, selectivity, linearity, accuracy and precision. The calibration curve was linear over the range of 5-2000 ng mL-1of donepezil with detection limit of 1.5 ng mL-1. Intra- and inter-day relative standard deviations were less than 2.5 %. The method was found to be suitable for quality control of donepezil hydrochloride in bulk drug as well as in human plasma.

Liquid-chromatographic assay of ibuprofen enantiomers in plasma.

1988 ◽  
Vol 34 (3) ◽  
pp. 493-496 ◽  
Author(s):  
R Mehvar ◽  
F Jamali ◽  
F M Pasutto
Keyword(s):  
Ambient Temperature ◽  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Ethyl Chloroformate ◽  
Organic Layer ◽  
Pharmacokinetic Studies ◽  
Sequential Reaction ◽  
Liquid Chromatographic

Abstract This stereospecific "high-performance" liquid-chromatographic (HPLC) assay is suitable for pharmacokinetic studies of ibuprofen (IB). Very efficient extraction of the drug and internal standard, (+/-)-2-(4-benzoylphenyl)butyric acid, from plasma with isooctane/isopropanol (95/5, by vol) is followed by sequential reaction of the enantiomers with ethyl chloroformate and (S)-(-)-1-(1-naphthyl)ethylamine. The reactions take place at ambient temperature in less than 4 min. The naphthylethylamide derivatives of IB enantiomers and internal standard are then extracted into chloroform. After the organic layer is evaporated, the reconstituted residue is chromatographed at ambient temperature on a C18 reversed-phase column with a mobile phase of acetonitrile/water/acetic acid/triethylamine (55/45/0.1/0.02 by vol) at a flow rate of 1 mL/min. The IB diastereoisomers, detected at 232 nm, are free of interfering peaks and have a resolution factor of 2.2. Within the examined enantiomer concentration range of 0.1 to 20 mg/L in plasma, the peak-area ratios varied linearly with the corresponding IB concentrations. We used the assay to study the pharmacokinetics of IB enantiomers in plasma of a subject who took a single 600-mg dose of racemic drug.

scholarly journals Analysis of morphine, morphine-3-glucuronide, morphine-6-glucuronide, codeine and codeine-6-glucuronide using HPLC: تحليل المورفين، المورفين -3 غلوكورونيد، المورفين -6-غلوكورونيد، الكودايين والكودايين -6-الغلوكورونيد باستخدام جهاز الفصل السائل عالي الكفاءة

2020 ◽  
Vol 4 (1) ◽  
Author(s):  
Abdullataif Aaied Almoterie, Mohammad Suliman Alshugeer, Abd
Keyword(s):  
High Performance ◽  
Direct Detection ◽  
Parent Compound ◽  
Internal Standard ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Stable Form ◽  
Uv Detector

In interpretive forensic and clinical toxicology, there is a great need for the identification and detection of opiate drugs and their various glucuronide metabolites. Glucuronides are usually determined by cleavage of the glucuronide bond with an enzyme (e.g., β-glucuronidase) or acid hydrolysis to yield the parent compound, which is subsequently detected. For Gas chromatography-mass spectrometry (GC-MS) analysis this may be via derivatization to a more volatile or stable form. Direct detection of the glucuronide conjugates overcomes the critical limitations of these approaches. In this conduct, a rapid and selective reversed-phase high-performance liquid chromatographic (HPLC) assay with gradient elution and ultraviolet detection for morphine, morphine-3-glucuronide, morphine-6-glucuronide, codeine, codeine-6-glucuronide and hydrocodone was developed. The separation was performed on a gemini C18 (Octadecyl carbon chain) analytical column (150  2.0 mm, 5 µm) and detected by an ultraviolet (UV) detector at 210 nm. The mobile phase consisted of an acetonitrile–phosphate buffer (0.0125 M, pH 7.5) with elution in the gradient mode ranging from 7.5–60% acetonitrile over 25 minutes (min) with a 0.2 mL/min flow rate. The calibration curves were linear (R2 range 0.997–0.999) in the concentration range 0.025–2 µg/mL for all analytes, using hydrocodone as the internal standard.  Therefore, this conduct aims to develop an efficient method of separation of morphine, codeine and glucuronides by HPLC-UV and to evaluate the use of SPME LC tips for the extraction of morphine, codeine and glucuronides from urine samples.

ICH/FDA Guidelines-Compliant Validated Stability-Indicating HPLC-UV Method for the Determination of Axitinib in Bulk and Dosage Forms

2020 ◽  
Vol 16 (8) ◽  
pp. 1106-1112
Author(s):  
Ibrahim A. Darwish ◽  
Nasr Y. Khalil ◽  
Mohammad AlZeer
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Degradation Products ◽  
Internal Standard ◽  
Dosage Forms ◽  
Uv Detector ◽  
Stability Indicating ◽  
Therapeutic Benefits ◽  
Relative Standard

Background: Axitinib (AXT) is a member of the new generation of the kinase inhibitor indicated for the treatment of advanced renal cell carcinoma. Its therapeutic benefits depend on assuring the good-quality of its dosage forms in terms of content and stability of the pharmaceutically active ingredient. Objective: This study was devoted to the development of a simple, sensitive and accurate stabilityindicating high-performance liquid chromatographic method with ultraviolet detection (HPLC-UV) for the determination of AXT in its bulk and dosage forms. Methods: Waters HPLC system was used. The chromatographic separation of AXT, internal standard (olaparib), and degradation products were performed on the Nucleosil CN column (250 × 4.6 mm, 5 μm). The mobile phase consisted of water:acetonitrile:methanol (40:40:20, v/v/v) with a flow rate of 1 ml/min, and the UV detector was set at 225 nm. AXT was subjected to different accelerated stress conditions and the degradation products, when any, were completely resolved from the intact AXT. Results: The method was linear (r = 0.9998) in the concentration range of 5-50 μg/ml. The limits of detection and quantitation were 0.85 and 2.57 μg/ml, respectively. The accuracy of the method, measured as recovery, was in the range of 98.0-103.6% with relative standard deviations in the range of 0.06-3.43%. The results of stability testing revealed that AXT was mostly stable in neutral and oxidative conditions; however, it was unstable in alkaline and acidic conditions. The kinetics of degradation were studied, and the kinetic rate constants were determined. The proposed method was successfully applied for the determination of AXT in bulk drug and dosage forms. Conclusions: A stability-indicating HPLC-UV method was developed and validated for assessing AXT stability in its bulk and dosage forms. The method met the regulatory requirements of the International Conference on Harmonization (ICH) and the Food and Drug Administration (FDA). The results demonstrated that the method would have great value when applied in quality control and stability studies for AXT.

Development of an HPLC method for measuring orally administered 1-substituted 2-alkyl-3-hydroxypyrid-4-one iron chelators in biological fluids

1990 ◽  
Vol 36 (1) ◽  
pp. 5-8 ◽  
Author(s):  
J G Goddard ◽  
G J Kontoghiorghes
Keyword(s):  
High Performance ◽  
Biological Fluids ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Iron Chelators ◽  
Serum Samples ◽  
Thalassemic Patient ◽  
Serum And Urine

Abstract "High-performance" liquid-chromatographic (HPLC) methods have been developed for identifying 1-substituted 2-alkyl-3-hydroxypyrid-4-one iron chelators in serum and urine. Ion pairing with heptane- or octanesulfonic acid in pH 2.0-2.2 phosphate buffer and reversed-phase chromatography were required to separate these compounds from endogenous compounds in both biological fluids. In both the 2-methyl and 2-ethyl series of 1-substituted compounds (H, methyl, ethyl, or propyl) the elution times increased in accordance with the n-octanol/water partition coefficients (propyl greater than ethyl greater than H greater than methyl). Urine samples were filtered (0.4 microns pore size) and injected either undiluted or after dilution with elution buffer. After the addition of internal standard, the plasma or serum samples were deproteinized by treatment with HCIO4, 0.5 mol/L, centrifuged, and the supernates were injected directly onto the HPLC. Using these procedures, we could identify 1,2-dimethyl-3-hydroxypyrid-4-one (L1) in the serum and urine of a thalassemic patient who had received a 3-g dose of the drug and in the urine of other patients who had received the same dose. One or more possible metabolites were also observed in the chromatograms of both urine and serum. The 24-h urinary output of L1 (0.22-2.37 g) and iron (10.6-71.5 mg) varied but there was no correlation between the two with respect to quantity or concentration. Instead, urinary iron output was higher in patients with a greater number of transfused units of erythrocytes. This is the first study in humans to show that L1 is absorbed from the gut, enters the circulation, and is excreted in the urine.

scholarly journals Determination of Finasteride in Tablets by High Performance Liquid Chromatography

2007 ◽  
Vol 4 (1) ◽  
pp. 109-116 ◽  
Author(s):  
K. Basavaiah ◽  
B. C. Somashekar
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Calibration Graph ◽  
Official Method ◽  
Pharmaceutical Dosage Forms ◽  
Bulk Drug ◽  
Liquid Chromatographic

A rapid, highly sensitive high performance liquid chromatographic method has been developed for the determination of finasteride(FNS) in bulk drug and in tablets. FNS was eluted from a ODS C18reversed phase column at laboratory temperature (30 ± 2°C) with a mobile phase consisting of methanol and water (80+20) at a flow rate of 1 mL min-1with UV detection at 225 nm. The retention time was ∼ 6.1 min and each analysis took not more than 10 min. Quantitation was achieved by measurement of peak area without using any internal standard. Calibration graph was linear from 2.0 to 30 μg mL-1with limits of detection (LOD) and quantification (LOQ) being 0.2 and 0.6 μg mL-1, respectively. The method was validated according to the current ICH guidelines. Within-day co efficients of variation (CV) ranged from 0.31 to 0.69% and between-day CV were in the range 1.2-3.2%. Recovery of FNS from the pharmaceutical dosage forms ranged from 97.89 – 102.9 with CV of 1.41-4.13%. The developed method was compared with the official method for FNS determination in its tablet forms.

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