scholarly journals Determination of five sulfonamides in medicated feedingstuffs by liquid chromatography with ultraviolet detection

2013 ◽  
Vol 57 (4) ◽  
pp. 545-552 ◽  
Author(s):  
Wojciech Jerzy Pietroń ◽  
Wojciech Cybulski ◽  
Dorota Krasucka ◽  
Agata Mitura ◽  
Katarzyna Kos ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Analytical Procedure ◽  
Mobile Phase Composition ◽  
Easy Method ◽  
Ultraviolet Detection ◽  
The Matrix ◽  
The Mean ◽  
Sensitivity Specificity

Abstract A fast and reliable method of liquid chromatography and ultraviolet detection of sulfaguanidine, sulfadiazine, sulfamethazine, sulfamethizole, and sulfamethoxazole in feedingstuffs was described. The method involves THE procedure of preparation of spiked samples, and extraction of sulphonamides from the matrix using a mixture of methanol and acetonitrile, followed by drying the extract and dissolving it in a phosphate buffer. The analysis uses octadecyl (C18) analytical column with UV detection at λ = 260 nm and a gradient programme of mobile phase composition. The analytical procedure has been successfully adopted and validated for quantitative determination of the sulfonamides in feedingstuff samples. Validation included sensitivity, specificity, linearity, repeatability, and intra-laboratory reproducibility. The mean recovery of sulfonamides was 84%, within the working range of 200-2000 mg/kg. Direct, simple sample preparation and HPLC-UV analysis allow the method to be successfully included in the scope of routine analyses. The presented results could be an answer to a need of simple and easy method for sulfonamide determination applicable in medicated feedingstuffs analysis.

scholarly journals Amphenicols stability in medicated feed – development and validation of liquid chromatography method

2014 ◽  
Vol 58 (4) ◽  
pp. 621-629 ◽  
Author(s):  
Wojciech Jerzy Pietro ◽  
Aneta Woźniak ◽  
Katarzyna Pasik ◽  
Wojciech Cybulski ◽  
Dorota Krasucka
Keyword(s):  
Liquid Chromatography ◽  
Analytical Procedure ◽  
Chromatography Method ◽  
The Matrix ◽  
The Mean ◽  
Liquid Chromatography Method ◽  
Sensitivity Specificity ◽  
Development And Validation ◽  
Feed Samples

Abstract A liquid chromatography-ultraviolet detection method for the determination of florfenicol (FF) and thiamphenicol (TAP) in feeds is presented. The method comprises the extraction of analytes from the matrix with a mixture of methanol and acetonitrile, drying of the extract, and its dissolution in phosphate buffer. The analysis was performed with a gradient programme of the mobile phase composed of acetonitrile and buffer (pH = 7.3) on a Zorbax Eclipse Plus C18 (150 × 4.6 mm, 5 μm) analytical column with UV (λ = 220 nm) detection. The analytical procedure has been successfully adopted and validated for quantitative determination of florfenicol and thiamphenicol in feed samples. Sensitivity, specificity, linearity, repeatability, and intralaboratory reproducibility were included in the validation. The mean recovery of amphenicols was 93.5% within the working range of 50-4000 mg/kg. Simultaneous determination of chloramphenicol, which is banned in the feed, was also included within the same procedure of FF and TAP stability studies. Storing the medicated feed at room temperature for up to one month decreased concentration in the investigated drugs even by 45%. These findings are relevant to successful provision of therapy to animals.

scholarly journals Determination of Tiamulin in Type C Medicated Swine Feeds Using High Throughput Extraction with Liquid Chromatography

2002 ◽  
Vol 85 (3) ◽  
pp. 533-540 ◽  
Author(s):  
Douglas B Moore ◽  
Nancy L Britton ◽  
Robert L Smallidge ◽  
Ken L Riter
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Test Results ◽  
Improved Method ◽  
Mobile Phase Composition ◽  
Significance Level ◽  
Paired Sample ◽  
Recovery Study ◽  
Type C

Abstract An improved method for extraction and analysis of tiamulin is presented to address issues that arose during routine analysis of Type C medicated swine feeds under the current U.S. Food and Drug Administration-Center for Veterinary Medicine (FDA-CVM) approved method. The issues included the need for higher sample throughput and the ability to accommodate a wider variety of feed matrixes. Changes to the FDA-CVM approved method include reduced sample size and solvent volumes, phosphate buffering of tartaric acid, centrifugation, and use of a new liquid chromatography column and adjusted mobile phase composition. A paired sample study was performed to compare performance of the new and existing methods. The paired sample study showed no statistical difference between sample means of paired sets of 17 samples analyzed by both methods (t = 1.95 at 0.05 significance level, p = 0.068). A recovery study showed the method precision to be 2.06% (coefficient of variation) with an average standard recovery of 95.8%. Ruggedness test results indicated good overall ruggedness of the method.

A Novel LC-MS Method for the Determination of Abiraterone in Rat Plasma and its Application to Pharmacokinetic Studies

2021 ◽  
Vol 17 ◽  
Author(s):  
Linzhi Dai ◽  
Pei Lv ◽  
Yun He ◽  
Xiaoli Wang ◽  
Lili Chen ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Analytical Procedure ◽  
Internal Standard ◽  
Rat Plasma ◽  
Pharmacokinetic Studies ◽  
Quadrupole Mass ◽  
Limit Of Quantitation

Background: High–performance liquid chromatography (HPLC)–ultraviolet (UV) and liquid chromatography (LC)–mass spectrometry (MS)/MS methods have been used to analyse abiraterone (ART); however, a single-quadrupole mass spectrometer with LC-MS systems has never been used to analyse ART. Objective: The study aimed to establish a novel, simple assay of quantitating ART in rat plasma through LC–MS. Method: The analytical procedure involved the extraction of ART and D4-ART (internal standard, IS) from rat plasma through simple protein precipitation. Chromatographic separation was achieved using an isocratic mobile phase (acetonitrile: 5 mM ammonium formate with 0.1% formic acid, 50:50 v/v) at a flow rate of 0.30 mL/min on a Waters XBridge® C18 column with a total run time of 5 min. LC–MS ion transitions monitored were 350.1 and 354.1 for ART and IS, respectively. The method was validated, and the results met acceptance criteria. Results: The lower limit of quantitation achieved was 1 ng/mL, and linearity was 1–8000 ng/mL. The intra- and inter-day precisions were 1.26%–14.20% and 5.49%–13.08%, respectively, in rat plasma.

scholarly journals Simultaneous Determination of Kynurenine and Kynurenic Acid by High-Performance Liquid Chromatography Photoirradiation System Using a Mobile Phase Containing 18-crown-6

2019 ◽  
Vol 12 ◽  
pp. 117864691983455
Author(s):  
Motomasa Atsumi ◽  
Ken-ichi Mawatari ◽  
Akari Morooka ◽  
Makoto Yasuda ◽  
Tomoko Fukuuchi ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Kynurenic Acid ◽  
Fluorometric Determination ◽  
The Mean

A high-performance liquid chromatography (HPLC) system has been developed for the fluorometric determination of kynurenine (KYN) and kynurenic acid (KYNA) in human serum using a mobile phase containing 18-crown-6. A retention time of KYNA was adjusted with pH of phosphate buffer in 18-crown-6. KYN and KYNA were separated on a CAPCELLPAK C18 (250 × 4.6 mm i.d.). The mobile phase consisted of 35 mmol/L phosphate buffer (pH 8.0)/methanol (85/15, v/v) containing 35 mmol/L hydrogen peroxide and 10 mmol/L 18-crown-6. The retention times of KYN and KYNA were 18and 24 minutes, respectively. The calibration graphs of KYN and KYNA were linear over the range 180 to 2900 and 1 to 84 nmol/L by injecting a 50-μL volume of KYN and KYNA, respectively. Pretreatment of serum was achieved by deproteinization only. The mean recoveries of KYN and KYNA from serum were more than 97%.

scholarly journals Determination of the Analgesic Components of Spasmomigraine® Tablet by Liquid Chromatography with Ultraviolet Detection

2007 ◽  
Vol 90 (1) ◽  
pp. 94-101 ◽  
Author(s):  
Fawzy A Elbarbry ◽  
Mokhtar M Mabrouk ◽  
Mohamed A El-Dawy
Keyword(s):  
Particle Size ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Ambient Temperature ◽  
Mobile Phase ◽  
High Performance ◽  
Internal Standard ◽  
Dosage Forms ◽  
Ultraviolet Detection

Abstract A procedure was developed for the determination of the analgesic components of Spasmomigraine® tablets, which are ergotamine (I), propyphenazone (II), caffeine (III), camylofin (IV), and mecloxamine (V). They were subjected to high-performance liquid chromatography on a column (300 × 3.9 mm, 10 μm particle size) packed with μ-Bondapak C18. Separations were achieved with the mobile phase methanol–water–triethylamine (60 + 40 + 0.1, v/v/v) flowing at a rate of 1.5 mL/min, and quantitative determination was performed at 254 nm at ambient temperature for I–III; acetonitrile–25 mM KH2PO4–acetic acid (45 + 55 + 0.2, v/v/v), flowing at a rate of 1.5 mL/min and detection at 234 nm at ambient temperature, was used for IV and V. Methyl paraben was used as an internal standard. The detection limits were 0.35 (I), 5.0 (II), 1.5 (III), 3.0 (IV), and 2.0 g/mL (V). The method was accurate (mean recovery 98 ± 2%, n = 4) and precise (coefficient of variation <5%, n = 5). The proposed method is rapid and sensitive and, therefore, suitable for the routine control of these ingredients in multicomponent dosage forms.

scholarly journals Determination of Chlorpheniramine Maleate and Tincture Ipecac in Dosage Form by Liquid Chromatography with Ultraviolet Detection

2003 ◽  
Vol 86 (4) ◽  
pp. 675-680 ◽  
Author(s):  
Mohamed A Eldawy ◽  
Mokhtar M Mabrouk ◽  
Fawzy A El-Barbary
Keyword(s):  
Liquid Chromatography ◽  
Dosage Form ◽  
Internal Standard ◽  
Reversed Phase ◽  
Chlorpheniramine Maleate ◽  
Ultraviolet Detection ◽  
British Pharmacopoeia ◽  
Phase Liquid ◽  
The Mean

Abstract A procedure was developed and validated for measuring chlorpheniramine maleate and tincture ipecac (as emetine hydrochloride) by reversed-phase liquid chromatography with methanol–10mM sodium heptanesulfonate (20 + 30) as the mobile phase; the pH was adjusted to 4 with acetic acid, and the flow rate was at 1.5 mL/min, with ultraviolet detection at 254 nm. Propyl paraben was used as the internal standard. The standard curves were linear (r = 0.998 and 0.9998) for both chlorpheniramine maleate and emetine hydrochlo-ride over the ranges of 5–100 and 0.1–40 μg/mL, respectively. The mean recoveries ± standard deviation were 101.37 ± 2.77% for chlorpheniramine maleate and 98.8 ± 1.47% for emetine hydrochlo-ride. The proposed method was applied to the determination of chlorpheniramine maleate alone in tablet and syrup dosage forms. The method also was applied to the determination of the emetine content of ipecac liquid extract and tincture ipecac; the results were compared with those of the method of the British Pharmacopoeia. The proposed method was applied successfully to the simultaneous determination of chlorpheniramine maleate and tincture ipecac, as emetine hydrochlo-ride, in syrup dosage form. Both drugs and the internal standard were separated from all interfering components in <5 min. The proposed method is simple, specific, and economical, when compared with other published methods that determine each component alone.

scholarly journals Simultaneous Determination of Six Triazolic Pesticide Residues in Apple and Pear Pulps by Liquid Chromatography with Ultraviolet Diode Array Detection

2001 ◽  
Vol 84 (5) ◽  
pp. 1543-1550 ◽  
Author(s):  
Carlo Bicchi ◽  
Chiara Cordero ◽  
Patrizia Rubiolo ◽  
Alessandro Occelli
Keyword(s):  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Pesticide Residues ◽  
Mobile Phase ◽  
Solid Phase ◽  
Diode Array ◽  
Diode Array Detection ◽  
Ultraviolet Detection ◽  
Array Detection

Abstract A method is described for the simultaneous determination of diclobutrazol, flusilazole, flutriafol, hexaconazole, paclobutrazol, and tetraconazole in apple and pear pulps used in baby food at a limit of 0.01 mg/kg. Apple and pear pulp samples are subjected to selective solid-phase microdispersion (SPMD) with SPE-ED Matrix-38 and acetone–cyclohexane, and the extracts are cleaned up on a Florisil cartridge with hexane–cyclohexane–acetone. The extracts are then analyzed by liquid chromatography with ultraviolet detection, using an octadecylsilane column with a gradient-programmed acetonitrile–water mobile phase. Recoveries were determined by spiking apple and pear pulps with the 6 pesticides under investigation at 0.1, 0.05, 0.03, and 0.01 mg/kg. Six determinations were performed at each level for each pesticide. Recoveries were ≥70% at the 0.01 mg/kg level.

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