饲料中四环素类药物含量的高效液相色谱测定

Simultaneous Determination of Multiple Tetracyclines in Feedstuff by High Performance Liquid Chromatography

建立了高效液相色谱法测定饲料中四环素类药物含量的方法：样品经甲醇一盐酸溶液提取，Waters Oasis HLB固相萃取柱净化，进行HPLC分析。标准校正曲线线性范围为0．05～2、0mg／L，相关系数r〉0．999。饲料中土霉素、四环素、金霉素和强力霉素的定量下限（LOQ）依次是2、0、2．0、4、0和4、0mg／kg；不同添加水平样品加标回收率为78％～103％，RSD小于11％。

A SPE -HPLC method for the simultaneous determination of multiple tetracyclines （TCs） residues in feedstuff was established. TCs in 1 g of feedstuff sample was extracted with 40 mL CH3OH - HC1, after centrifugation, 1 mL of the supernatant liquid was cleaned with a Waters Oasis HLB SPE cartridge, and then detected by HPLC. The calibration curve was linear in the range 0.05 - 2.0 mg/kg and r 〉0. 999. The limit of quantification（LOQ） was 0. 025, 0. 025, 0. 05 and 0. 05 mg/kg and the recovery rates were 78% - 103% with RSD 〈 11% at the spiking level 2. 0, 2.0, 4.0 and 4.0 mg/L, respectively, for oxytetracyline, tetracycline, chlortetracycline and doxytetracyline in feedstuff. The method was suitable for the detection of TCs residues in feedstuff.