Determination of Oxytetracycline from Salmon Muscle and Skin by Derivative Spectrophotometry

被引:6
|
作者
Toral, M. Ines [1 ]
Sabay, Tamara [1 ]
Orellana, Sandra L. [2 ]
Richter, Pablo [3 ]
机构
[1] Univ Chile, Fac Sci, Dept Chem, Santiago, Chile
[2] Univ Austral Chile, Inst Chem Sci, Fac Sci, Valdivia, Chile
[3] Univ Chile, Dept Chem, Dept Inorgan & Analyt Chem, Fac Chem & Pharmaceut Sci, Santiago, Chile
关键词
PERFORMANCE LIQUID-CHROMATOGRAPHY; FLUORESCENCE DETECTION; TETRACYCLINE ANTIBIOTICS; RESIDUES; AQUACULTURE; SAMPLES;
D O I
10.5740/jaoacint.14-027
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A method was developed for the identification and quantification of oxytetracycline residues present in salmon muscle and skin using UV-Vis derivative spectrophotometry. With this method, it was possible to reduce the number of steps in the procedure typically required for instrumental analysis of a sample. The spectral variables, order of the derivative, scale factor, smoothing factor, and analytical wavelength were optimized using standard solutions of oxytetracycline dissolved in 900 mg/L oxalic acid in methanol. The matrix effect was significant; therefore, quantification for oxytetracycline residues was carried out using drug-free salmon muscle and skin samples fortified with oxytetracycline. The LOD and LOQ were found to be 271 and 903 mu g/kg, respectively. The precision and accuracy of the method were validated using drug-free salmon muscle and skin tissues fortified at three different concentrations (8, 16, and 32 mg/kg) on 3 different days. The recoveries at all fortified concentrations were between 90 and 105%, and RSDs in all cases were less than 6.5%. This method can be used to screen out compliant samples and thereby reduce the number of suspect positive samples that will require further confirmatory analysis.
引用
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页码:559 / 565
页数:7
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