Simultaneous HPLC Assay of Gliclazide and Ciprofloxacin in Plasma and its Implementation for Pharmacokinetic Study in Rats

2021 ◽  
Author(s):  
Lucy Sasongko ◽  
Gladdis K Pratiwi ◽  
Margaretha Leo ◽  
Jeffry Adiwidjaja
Keyword(s):  
High Performance ◽  
Plasma Sample ◽  
Pharmacokinetic Interaction ◽  
Gradient Elution ◽  
Interaction Study ◽  
Total Flow ◽  
Total Flow Rate ◽  
Chromatography Method ◽  
Ultraviolet Detector ◽  
Liquid Chromatography Method

Abstract A simple and reliable high-performance liquid chromatography method for simultaneous quantitation of gliclazide and ciprofloxacin in plasma sample has been developed and validated. This method implements protein precipitation, a simple and practical pretreatment method by the addition of acetonitrile that gives a clean supernatant. The separation was carried out in a system consisted of a C18 column with acetonitrile and KH2PO4 (0.01 M, 0.1% v/v of triethylamine, pH 2.7) as the mobile phase in a gradient elution at a total flow-rate of 1 mL/min. Gliclazide and ciprofloxacin were quantitated using an ultraviolet detector set at wavelengths of 229 and 277 nm, respectively, which ensures optimal sensitivity for both compounds. This method possesses an excellent linearity at concentration ranges of 0.5–50 mg/L for gliclazide and 0.1–10 mg/L for ciprofloxacin. High within- and between-run accuracy for both gliclazide (% error of −8.00 to 0.45%) and ciprofloxacin (% error of −10.00 to 7.63%) were demonstrated. The intra- and inter-day precision (expressed as %CV) was <8 and 12% for gliclazide and ciprofloxacin, respectively. Both analytes were stable during storage and sample processing. The method reported in this study can be implemented for pharmacokinetic interaction study in rats.

scholarly journals Fluoroquinolone residues in raw cow’s milk

2011 ◽  
Vol 29 (No. 6) ◽  
pp. 641-646 ◽  
Author(s):  
P. Navrátilová ◽  
I. Borkovcová ◽  
J. Vyhnálková ◽  
L. Vorlová
Keyword(s):  
High Performance ◽  
Raw Milk ◽  
Gradient Elution ◽  
Maximum Residue Limit ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Milk Products ◽  
Milk Samples ◽  
Efficient Control ◽  
Liquid Chromatography Method

The aim of the study was to monitore the levels of fluoroquinolone residues in bulk samples of raw cow’s milk. The bulk samples of raw cow’s milk (n = 150) were obtained from 58 different milk suppliers in the South Moravian and Vysočina Regions. The samples were analysed by reverse phase high-performance liquid chromatography method with fluorescence detection and gradient elution. 87.3% of the raw milk samples were positive for the fluoroquinolones residues. Flumequine was present in none of the samples. The levels of other fluoroquinolones investigated were below the recommended maximum residue limit. The results of the study indicate that fluoroquinolones are frequently administered to the dairy cows in spite of the recommendations of CVMP. The most frequently determined was enrofloxacin and its indicator residue, i.e. ciprofloxacin. An efficient control of the veterinary drugs residues in milk is very important to ensure the safety of the milk and milk products.

scholarly journals Determination of Chlorotetracycline and Doxycycline in Medicated Feedingstuffs by Liquid Chromatography

2012 ◽  
Vol 56 (3) ◽  
pp. 329-333 ◽  
Author(s):  
Ewelina Patyra ◽  
Ewelina Kowalczyk ◽  
Krzysztof Kwiatek
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Analytical Procedure ◽  
Solid Phase ◽  
Gradient Elution ◽  
Diode Array ◽  
Chromatography Method ◽  
Array Detection ◽  
Liquid Chromatography Method

Abstract High performance liquid chromatography method with diode array detection (HPLC-DAD) was developed and optimised for the determination of tetracyclines (TCs) in medicated feedingstuffs. The extraction of the analyte from feedingstuffs was performed with Na2EDTA-McIlvaine buffer (pH 2.5 and pH 4). The extracts were cleaned up by solid phase extraction using octadecyl cartridges (C18). The samples were dried up and redissolved in the mixture of oxalic acid and methanol. Separation was performed on reserved phase column (Phenomenex C18, 250 x 4.6 mm, 5 μm) by multistep gradient elution, which provided better chromatographic separation. The analysis was performed at a wavelength of 390 nm. Validation study of the method revealed that all obtained calibration curves showed good linearity R= 0.9985 for doxycycline (DC) and R= 0.9981 for chlorotetracycline (CTC) over the range of 25-2,000 mg/kg. The analytical procedure was successfully adapted for quantitative determination of DC and CTC in medicated feedingstuff samples. Validation included determination of specificity, linearity, and repeatability. Mean recovery for spiked samples was 93.1% for CTC and 93.2% for DC. The results of validation of the analytical procedure proved that presented method is efficient, precise and useful for quantification of DC and CTC in medicated feedingstuffs.

scholarly journals Development and Validation of a Stability-Indicating High-Performance Liquid Chromatography Method for the Simultaneous Determination of Albuterol, Budesonide, and Ipratropium Bromide in Compounded Nebulizer Solutions

2011 ◽  
Vol 94 (1) ◽  
pp. 110-117 ◽  
Author(s):  
Anthony J Blewett ◽  
Deepti Varma ◽  
Tiffany Gilles ◽  
Rashidi Butcher ◽  
Jaini Jacob ◽  
...  
Keyword(s):  
High Performance ◽  
Ipratropium Bromide ◽  
Gradient Elution ◽  
Chromatography Method ◽  
Alkali Solutions ◽  
Ensure Patient Safety ◽  
Liquid Chromatography Method ◽  
Development And Validation ◽  
Hydrolysis Of

Abstract In recent years, there has been a large increase in the use of pharmaceutical compounding to prepare medications that are not commercially available. The treatment of asthma typically includes the use of albuterol (ALB), ipratropium bromide (IPB), and/or budesonide (BUD) nebulizer solutions. There is currently no commercially available nebulizer solution containing all three of these compounds, and patients must rely on often-unregulated compounding. There is a distinct need for methodologies that can be used to analyze compounded formulations to ensure patient safety. We report an HPLC-UV method to separate and quantitate ALB, IPB, and BUD in nebulizer solutions. The method used a gradient elution to achieve separation via an RP C18 column. The method was validated, showed good selectivity, and was linear over several orders of magnitude. The method was applied to the analysis of nebulizer solutions and determination of their storage stability. Significant ALB-dependent degradation occurred within 5 h in solutions formulated with the free base of ALB, while those containing the sulfate salt of ALB produced no degradation. Alkali solutions can cause base-catalyzed hydrolysis of IPB and degradation of BUD. Compounded formulations containing ALB need to include an acid to control pH and prevent degradation.

Quantification of Pyrazinamide in Human Plasma by Validated High Performance Liquid Chromatography Method

2021 ◽  
Vol 15 (10) ◽  
pp. 2896-2899
Author(s):  
Waleed Arshad ◽  
Naseem Saud Ahmad ◽  
Abdul Muqeet Khan ◽  
Iram Imran ◽  
Qura- Tul-Ain ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
Ultra Violet ◽  
Chromatography Method ◽  
Ultraviolet Detector ◽  
Relative Standard ◽  
Liquid Chromatography Method

Objective: To be able to accurately determine the quantity of Pyrazinamide (PZA) in different tablet preparations and human plasma using an Ultra violet detector equipped high performance liquid chromatography (HPLC). Study Design: Experimental study Place and Duration of Study: Department of Bioequivalence Studies, University of Veterinary and Animal Sciences Lahore and the Department of Pharmacology, University of Health Sciences, Lahore the from 1st April 2017 to 31st March 2018. Methodology: Two mobile phases were used, the first compromised of disodium hydrogen phosphate buffer having a pH of 6.8 and acetonitrile in the proportion of (95:5) and the second was a combination of aforesaid substances in equivalent proportion (50:50 v/v). The gradient for the first 5 min was exclusively Mobile phase “a” after which 5-6 min Mobile phase “b” was raised from 0 to 100% and was kept at 100% till the completion of the cycle. The flow of mobile phase was kept at 1000 µl/min. Determination of PZA was done using a ultraviolet detector at a wavelength of 238 nm. Amount of sample injected was 40 μl. Procedure was done by using Shizmadu Chromatographic System, Japan equipped with a SIL-20AC HT auto-sampler, SPD-M20A, CTO 20 AC, a LC-20AT VP pump, and CBM 20A controller unit. A C18 column was used as well. Results: Retention time of PZA was 6.1±2%. Precision was 0.46 to 2.20% relative standard deviation for intra assay and for inter assay we obtained 0.29 to 34.45% RSD for all quality control levels. The overall recovery of PZA was 96.75%. Conclusion: High selectivity for PZA was seen and no other spikes from drugs present in FDC regimen were observed at the time when PZA is detected in blank plasma samples Key words: Chromatography, High pressure liquid. Pyrazinamide. Tuberculosis

scholarly journals Forced degradation of tacrolimus and the development of a UHPLC method for impurities determination

2019 ◽  
Vol 69 (3) ◽  
pp. 363-380 ◽  
Author(s):  
Tanja Rozman Peterka ◽  
Tina Trdan Lušin ◽  
Jure Bergles ◽  
Zoran Ham ◽  
Rok Grahek ◽  
...  
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
Dosage Forms ◽  
Forced Degradation ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Forms ◽  
Thermal Light ◽  
Forced Degradation Studies ◽  
Degradation Studies ◽  
Liquid Chromatography Method

Abstract An ultra-high performance liquid chromatography method for simultaneous determination of tacrolimus impurities in pharmaceutical dosage forms has been developed. Appropriate chromatographic separation was achieved on a BEH C18 column using gradient elution with a total run time of 14 min. The method was applied to analyses of commercial samples and was validated in terms of linearity, precision, accuracy, sensitivity and specificity. It was found to be linear, precise and accurate in the range of 0.05 to 0.6 % of the impurities level in pharmaceutical dosage forms. Stability indicating power of the method was demonstrated by the results of forced degradation studies. The forced degradation study in solution revealed tacrolimus instability under stress alkaline, thermal, light and photolytic conditions and in the presence of a radical initiator or metal ions. The drug was stable at pH 3–5. Solid-state degradation studies conducted on amorphous tacrolimus demonstrated its sensitivity to light, elevated temperature, humidity and oxidation.

Determination of Fluoroquinolones Residual in Freshwater Fish by HPLC

2014 ◽  
Vol 1033-1034 ◽  
pp. 634-637
Author(s):  
Yue Jin ◽  
Wen Yu Zhang ◽  
Qian Wang ◽  
Yi Qing Yang ◽  
Li Ya Liang ◽  
...  
Keyword(s):  
Freshwater Fish ◽  
High Performance ◽  
High Efficiency ◽  
Solid Phase ◽  
Gradient Elution ◽  
Extraction Column ◽  
Uv Detector ◽  
Chromatography Method ◽  
Phase Gradient ◽  
Liquid Chromatography Method

HPLC (High Performance Liquid Chromatography) method for danofloxacin(DAN), enrofloxacin(ENR), sarafloxacin(SAR) and difloxacin(DIF) residues in freshwater fish was developed. The fish sample was extracted with methanol-water-acetic acid(2/8/0.01, V/V/V), performed on a C18 solid-phase extraction column. With methanol+malonic acid-magnesium chloride aqueous solution as mobile phase, gradient elution at 30°C, inject volume was 20μL. The wavelength of UV detector was 280 nm. The linear rang of four drugs was 0.1~10μg/mL. In the level of 0.5μg/kg and 4.0μg/kg, the average recovery of the four kinds of drugs was 79.81%~92.03% , the RSD was 1.03%~4.07%. The limit of DAN, ENR, SAR, and DIF was 0.1μg/kg, 0.1μg/kg, 0.05μg/kg, and 0.05μg/kg individual. This method was employed to analyze freshwater fishes, such as catfish, chub and carp, because of its simplicity and high efficiency.

scholarly journals High Performance Liquid Chromatography Method for Determination of Trace Amount of Ibutilide Fumarate in Pharmaceutical Manufacturing Environments

2009 ◽  
Vol 6 (1) ◽  
pp. 53-60
Author(s):  
M. Satya Babu ◽  
Prathama S. Mainkar ◽  
Y. Anjaneyulu
Keyword(s):  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Active Pharmaceutical Ingredient ◽  
Gradient Elution ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Chromatography Method ◽  
Test Concentration ◽  
Liquid Chromatography Method ◽  
Manufacturing Environments

A rapid and sensitive RP-HPLC method with UV detection at 227 nm for routine analysis of washed MLs (mother liquors) from equipment after manufacturing and thereby cleaning of ibutilide fumarate active pharmaceutical ingredient was developed. Chromatography was performed with mobile phase containing a mixture of aqueous 0.01 M potassium dihydrogen phosphate (KH2PO4) and acetonitrile. The gradient elution was developed for better and optimized results. The developed method was validated for precision which includes system precision and method precision, accuracy, intra-day and using different system and finally linearity studies from 0.4 to 150%. The method is ascertained to be having good repeatability and reproducibility. The %RSD for method precision (5 different preparations at test concentration) was observed to be 1.36, wherein the system precision (6 repeated injections of same preparation) was observed to be 0.33. The % recovery from ‘Accuracy’ studies yielded the recovery of 99-100% which indicates the capability of the method. The linearity of the method was studied right from 0.4 to 150% which shows the method is quite linear with a correlation coefficient of 0.9998. The proposed method was simple, highly sensitive, precise, and accurate.The retention time less than 15 min, indicated that the method is useful for routine testing of washed MLs from equipment after manufacturing and cleaning of ibutilide fumarate.

scholarly journals Determination of eight lignans in Schisandra chinensis and Schisandra sphenanthera

2016 ◽  
Vol 11 ◽  
pp. S161-S167 ◽  
Author(s):  
Xu Guangyu ◽  
Niu Jiamu ◽  
Yuan Guangxin ◽  
Bai Yu ◽  
Li Hongyu ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Gradient Elution ◽  
Schisandra Chinensis ◽  
Chromatography Method ◽  
Schisandra Sphenanthera ◽  
Content Determination ◽  
Liquid Chromatography Method

A high performance liquid chromatography method for the determination of eight lignans contents in Schisandra chinensis and Schisandra sphenanthera was developed. The chromatographic column was Agilent ZORBAX 300SB-C18 column (4.6 mm × 250 mm?5 ?m). The mobile phase was methanol-water, a gradient elution was conducted and the detection wavelength was at 230 nm. The results showed that the recovery rate of eight lignans was 92.2-102.9% and RSD was 1.5-4.2%. The established content determination method was simple, sensitive, accurate and stable, and can be used to control the quality of S. chinensis and S. sphenanthera. 

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