高效液相色谱法测定肉、奶、鱼中螺旋霉素及其初级代谢物新螺旋霉素的含量

M. Horie, Y. Kido, M. Murayama, M. Toyoda, H. Nakazawa
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引用次数: 5

摘要

建立了高效液相色谱法测定肉类、鱼类和牛奶中螺旋霉素I(主要和最重要的成分)及其代谢物新螺旋霉素I的简便、快速方法。用1.2%偏磷酸-甲醇(5:5)提取药物,用Bond Elut SCX (500mg)药筒清洗。色谱柱为Puresil 5C18 (150×4.6mm),流动相为0.05mol/L磷酸缓冲液(pH 2.5) -乙腈(76:24),流速为0.5mL/min。药物在235nm处检测。两种药物的校准图在2 ~ 50ng范围内呈直线关系。在0.2μg/g水平下,三种药物的回收率为80.3 ~ 85.3%,两种药物的检出限均为0.05μg/g。
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Determination of Spiramycin I and Its Primary Metabolite Neospiramycin I in Meat, Milk and Fish by HPLC
A simple and rapid method using HPLC for the determination of spiramycin I (major and most important component) and its metabolite, neospiramycin I, in meat, fish and milk has been developed. Neospiramycin I was obtained by acidic treatment of spiramycin I. The drugs were extracted with 1.2% metaphosphoric acid-methanol (5:5), and the extracts were cleaned up on a Bond Elut SCX (500mg) cartridge. The HPLC separation was performed on a Puresil 5C18 column (150×4.6mm i. d.) using 0.05mol/L phosphate buffer (pH 2.5) -acetonitrile (76:24) as the mobile phase at a flow rate of 0.5mL/min. The drugs were detected at 235nm. The calibration graphs were rectilinear from 2 to 50ng for both drugs. The recoveries of the drugs from meat, milk and fish at the level of 0.2μg/g were 80.3-85.3%, and detection limits were 0.05μg/g for both drugs.
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