反相高效液相色谱测定动物源食品中大观霉素残留

Determination of spectinomycin residues in animal food by RP-HPLC

目的建立反相高效液相色谱法配合电化学检测器测定动物源食品中大观霉素残留。方法用三氯乙酸匀浆抽提以脱去试样中的蛋白，然后用二氯甲烷去除试样中的脂溶性物质，再经LC-SCX阳离子固相萃取小柱净化处理，产物进行检测。流动相为离子对缓冲体系（0.02mol／L柠檬酸：0．004mol／L庚烷磺酸钠，50％NaOH调pH至6．10）：乙腈（体积比为92．5：7．5），流速0.6ml／min，工作电极电压1．0V，柱温35℃，检测波长254nm。结果大观霉素在0．01-10．0μg／ml范围内线性关系良好，相关系数尺=0．99998。结论该法简便、直接、准确。

Objective A reversed-phase high performance liquid chromatography （RP-HPLC） method with electrochemical detector was established for the determination of spectinomycin residues in animal food. Methods The samples were deproteinized by trichloroacetic acid, and the fatty soluble substances were extracted with dichloromethane. Followed by cleaned-up on a LC-SCX positive ion solid-phase extraction column, then the extracts were determined. The mobile phase was citric acid ion-pair buffer solution （0. 02mol/L citric acid ： 0. 004mol/L sodium heptanesulfonate, the pH adjusted to 6.10 by 50% NaOH） ： acetonitrile （92.5 ： 7.5, V/V）. The flow rate was 0. 6ml/min, the working electrode voltage was 1.0V, the column temperature was maintained at 35℃, and the detection wavelength was at UV 254nm. Results The linear relationship of the peak and concentration of spectinomycin was determined as 0. 01- 10.0μg/ml, with a regression coefficient of 0. 99998. Conclusions The method is simple, direct,and accurate.