高效液相色谱法检测畜禽肉中四环素类药物残留的条件优化

对畜禽肉中四环素类残留的检测方法进行改进,选用Na2EDTA-McIlvaine缓冲溶液作为提取液进行超声提取,经C18固相萃取小柱净化,脱溶剂后用流动相三氟乙酸-乙腈溶解,使用高效液相色谱-PDA检测器分段采集355 nm及270 nm波长下的色谱信息,对前处理方法及色谱条件进行优化。四环素、土霉素在0.01～1μg/g范围内,金霉素、多西环素在0.02～2μg/g范围内回收率为60%～85%,相对标准偏差小于5%,可以满足国家残留限量0.1～0.6μg/g的检测要求。

OPTIMIZATION OF HIGH PERFORMANCE LIQUID CHROMATOGRAPHY FOR DETERMINATION OF FOUR KINDS OF TETRACYCLINES IN MEAT

A method for determination of the residues of four kinds of tetraeyelines in the meat of livestock and poultry was optimized. The four kinds of drugs such as tetracycline, oxytetracycline, chlortetracycline and doxycycline were extracted by Na2EDTA -McIlvaine buffer solution, purified by C18 SPE column, dissolved by mobile phase after desolvation, and determined by HPLC with PDA detector in segmented acquisition mode. The pretreating method and chromatograpy conditions were optimized. The results showed that the detection limits were 10 ng/g for tetracycline and oxytetracycline, 20 ng/g for chlortetracycline and doxycycline. The recoveries were in the ranges of 60% -85% with the relative standard deviation less than 5%. The method could satisfy the request of legislation on maximum residue limits in the range of 0.1 - 0.6 μg/g.