scholarly journals DETERMINATION OF VULCANIZATION ACCELERATORS IN ANALYSIS OF POLYMER MATERIALS BY HPLC

Author(s):  
A. V. Yukhnik ◽  
S. M. Leschev

A method of simultaneous determination of altax, captax, thiuram D, thiuram E, thimate and ethylthimate in aqueous extracts in the sanitary-chemical analysis by high performance liquid chromatography has been developed. Determination was based on the gradient separation of altax, captax, thiuram D, thiuram E, thimate, ethylthimate extracted by water from test objects using Waters XTerra MS C18 column of 250 mm length, internal diameter 4.6 mm, graining phase 5 μm, while UV detection wavelengths were 265 nm and 320 nm. Retention times were 10.3±0.2 min for altax, 3.6±0.2 min for captax, 9.0±0.2 min for thiuram D, 12.3±0.2 min for thiuram E, 11.0±0.2 min for thimate, 15.5±0.2 min for ethylthimate. It has been shown that the method is linear in the range of 0.05–0.60 mkg/ml for altax, 0.005–0.60 mkg/ml for captax, 0.005–0.75 mkg/ml for thiuram D and thiuram Е, 0.01–0.90 mkg/ml for thimate and ethylthimate. Using the calibration graph and standard deviations of analytical signal, following limits of quantification were calculated: 0.01 mkg/ml for altax, 0.002 mkg/ml for captax, 0.003 mkg/ml for thiuram D, 0.005 mkg/ml for thiuram Е, 0.01 mkg/ml for thimate and ethylthimate.

2010 ◽  
Vol 55 (2) ◽  
pp. 854-859 ◽  
Author(s):  
Kamil Uney ◽  
Feray Altan ◽  
Muammer Elmas

ABSTRACTCefquinome has a broad spectrum of antibacterial activity and was developed especially for use in animals. A simple and sensitive high-performance liquid chromatography (HPLC) method with UV-visible detection for quantification of cefquinome concentrations in sheep plasma was developed and validated. Separation of cefquinome from plasma components was achieved on a Phenomenex Gemini C18column (250 mm by 4.6 mm; internal diameter [i.d.], 5 μm). The mobile phase consisted of acetonitrile and 0.1% trifluoroacetic acid in water and was delivered at a rate of 0.9 ml/min. A simple and rapid sample preparation involved the addition of methanol to 200 μl of plasma to precipitate plasma proteins followed by direct injection of 50 μl of supernatant into the high-performance liquid chromatography system. The linearity range of the proposed method was 0.02 to 12 μg/ml. The intraday and interday coefficients of variation obtained from cefquinome were less than 5%, and biases ranged from −3.76% to 1.24%. Mean recovery based on low-, medium-, and high-quality control standards ranged between 92.0 and 93.9%. Plasma samples were found to be stable in various storage conditions (freeze-thaw, postpreparative, short-term, and long-term stability). The method described was found to be readily available, practicable, cheap, rapid, sensitive, precise, and accurate. It was successfully applied to the study of the pharmacokinetics of cefquinome in sheep. This method can be very useful and an alternate to performing pharmacokinetic studies in the determination of cefquinome for clinical use.


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