• 关键词：白萝卜  高效液相色谱  四环素  抗生素

• 基金项目：环保公益性行业科研专项(No.201009017);中央级公益性科研院所基本科研业务费专项资金(No.PM-ZX021-201211-102)

• 贺德春
• 环境保护部华南环境科学研究所, 广州 510655

• 许振成
• 环境保护部华南环境科学研究所, 广州 510655

• 吴根义
• 湖南农业大学资源与环境学院, 长沙 410128

• 刘庆
• 环境保护部华南环境科学研究所, 广州 510655

• 秦国建
• 湖南农业大学资源与环境学院, 长沙 410128

• 何金华
• 湖南农业大学资源与环境学院, 长沙 410128

• 摘要：建立了白萝卜中4种四环素类抗生素(土霉素、四环素、金霉素、强力霉素)的高效液相色谱测定法.样品用0.02 mol·L^-1的氯化镁-柠檬酸混合液提取2次,甲醇提取1次,甲醇提取液浓缩至干后用0.02 mol·L^-1的氯化镁与0.02 mol·L^-1柠檬酸混合溶液溶解残渣,合并3次提取液过Waters Oasis HLB固相小柱萃取,10 mL甲醇-乙酸乙酯(1:9,V/V)洗脱.以反相C18柱为分离柱,甲醇、乙腈、0.01 mol·L^-1草酸与0.01 mol·L^-1三氯乙酸为流动相进行梯度洗脱,11 min内分离4种抗生素.结果发现,在0.05~10.00 μg·mL^-1范围内,4种抗生素的峰面积与质量浓度的线性关系良好(R²≥0.999),土霉素、四环素、金霉素与强力霉素的定量限(LOQ)分别为2.9、4.3、8.9 和 5.2 μg·kg^-1;添加水平分别为10、100、1000 μg·kg^-1时,土霉素、四环素、金霉素与强力霉素的回收率分别在78.4%~88.8%、82.8%~92.4%、79.0%~83.0%和74.9%~84.5%之间,变异系数均小于8.9%.本方法成功用于实际样品的测定,结果表明,采集的样品中土霉素、四环素、金霉素和强力霉素的最大含量分别为53、41、79 和91 μg·kg^-1.

• Abstract：A method for the determination of four tetracyclines (oxytetracyline, tetracycline, chlortetracycline and doxytetracyline) from radish has been developed using high performance liquid chromatography with UV detector. The analytes were first extracted twice using a mixtural of 0.02 mol·L^-1 magnesium chloride and 0.02 mol·L^-1 citric acid and then once using methanol from radish. The extracts were cleaned-up and pre-concentrated by an HLB cartridge and then eluted by a mixture of methanol/ethyl acetate (1:9,V/V). Separation was performed on a reverse-phase Cl8 column with gradient elution using a mixed solution composed of methanol, Acetonitril, 0.01 mol·L^-1 oxalic acid and 0.01 mol·L^-1 trichloroacetic acid. The four antibiotics were separated within 11 min. The calibration curve was linear in the range 0.05~10.00 mg·L^-1 and R²>0.999. The limit of quantification (LOQ) was 2.9, 4.3, 8.9 and 5.2 μg·kg^-1 for oxytetracyline, tetracycline, chlortetracycline and doxytetracyline in radish. Recovery experiments were performed using spiked radish and concentrations varied from 10 to 1000 μg·kg^-1. The recovery rates for the oxytetracyline, tetracycline, chlortetracycline and doxytetracyline were 78.4%~88.8%, 82.8%~92.4%, 79.0%~83.0% and 74.9%~84.5% (RSD<8.9%, n=5), respectively. In radish samples, a maximum concentration of 53, 41, 79 and 91 μg·kg^-1 for oxytetracyline, tetracycline, chlortetracycline and doxytetracyline, respectively, were found. The method was suitable for the detection of tetracyclines residues in radish.

• Key words：radish  HPLC  tetracycline  antibiotics

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