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.

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.

Separation and Determination of Some Aromatic Sulfones by Reversed-Phase High-Performance Liquid Chromatography

1994 ◽  
Vol 59 (3) ◽  
pp. 569-574 ◽  
Author(s):  
Josef Královský ◽  
Marta Kalhousová ◽  
Petr Šlosar
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Uv Spectra ◽  
Optimum Conditions ◽  
Linear Calibration ◽  
Technical Grade

The reversed-phase high-performance liquid chromatography of some selected, industrially important aromatic sulfones has been investigated. The chromatographic behaviour of three groups of aromatic sulfones has been studied. The optimum conditions of separation and UV spectra of the sulfones and some of their hydroxy and benzyloxy derivatives are presented. The dependences of capacity factors vs methanol content in mobile phase are mentioned. The results obtained have been applied to the quantitative analysis of different technical-grade samples and isomer mixtures. For all the separation methods mentioned the concentration ranges of linear calibration curves have been determined.

Determination of adenine nucleotides by the modified method of high-performance liquid chromatography

2021 ◽  
Vol 66 (3) ◽  
pp. 172-176
Author(s):  
Lyubov Borisovna Kalikova ◽  
E. R. Boyko
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Adenine Nucleotides ◽  
Release Time ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Standard Solutions

Adenine nucleotides (ATP, ADP and AMP) play a central role in the regulation of metabolism and energy: they provide the energy balance of the cell, determine its redox state, act as allosteric effectors of a number of enzymes, modulate signaling and transcription factors and activate oxidation or biosynthesis substrates. A large number of methods have been developed to determine the level of ATP, ADP and AMP, but the most universal and effective method for the separation and analysis of complex mixtures is the reversed-phase high-performance liquid chromatography method (RP-HPLC). The aim of this study is to determine the optimal conditions for the qualitative separation and quantitative determination of standard solutions of ATP (1 mmol/l), ADP (0,5 mmol/l) and AMP (0,1 mmol/l) by RP-HPLC. The degree of separation of adenine nucleotides was estimated by the time of peak output in the chromatogram. To achieve the goal, the following tasks were set: assess the effect of the temperature of the analysis on the separation and change of the release time of the analytes in the chromatogram; determine the most optimal composition of the mobile phase for the separation of ATP, ADP and AMP in the chromatogram (the content of the organic solvent in the solution); to identify the effect of pH of the mobile phase on the separation of standard solutions of adenine nucleotides; set the optimal molarity of the mobile phase for the separation of ATP, ADP and AMP in the chromatogram. It was found that the temperature of the analysis does not affect the quality of peak separation, while the composition and pH of the mobile phase have a significant effect on the complete and clear separation of the studied nucleotides in the chromatogram. It was determined that the analysis temperature of 37°C and the mobile phase of 0.05 M KH2PO4 (pH 6.0) are optimal for separating the peaks of adenine nucleotides.

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