流动注射在线预富集-高效液相色谱法测定水产品中4种磺胺类药物

摘要

Using activated carbon fibre as the absorbent, a flow injection on-line preconcentration-high performance liquid chromatographic method for the determination of four kinds of sulfonamides (sulfathiazole, sulfamethazine, sulfamonomethoxine and sulfaquinoxaline) in aquatic products was established. The samples were extracted by phosphate buffer solution, then preconcentrated on activated carbon fibre by flow injection. The separation was carried out with an Eclipse XDB-C18 column (250 mm×4. 6 mm, 5 μm) in the mobile phase system of formic acid solution-formic acid methanol solution (60∶40, V/V) at pH = 3. 0, the flow rate was 1. 0 mL/min . The detection was performed at 270 nm wavelength. The experiment result showed that the good linear relationship was obtained in the sulfonamides concentrations from 0. 001 -0. 064 mg/L with the correlation coefficient from 0. 9997 to 0. 9999. The detection limit was 0. 48-1. 15 u.g/L(S/N=3). The enrichment factors for the four sulfonamides were from 137 to 406. The recoveries were 93. 5%-104. 0%. This method was easy to operate with precise result and good repetition and can be successfully applied to the determination of sulfathiazole, sulfamethazine, sulfamonomethoxine and sulfaquinoxaline.%建立了以活性碳纤维作吸附剂,流动注射在线预富集与高效液相色谱联用法测定水产品中4种磺胺类药物(磺胺噻唑、磺胺二甲嘧啶、磺胺间甲氧嘧啶、磺胺喹噁啉)残留含量的方法.样品经磷酸盐缓冲溶液提取后,采用活性碳纤维作吸附剂流动注射在线预富集,在pH 3.0的甲酸溶液-甲酸甲醇溶液(60∶40,V/V)的流动相体系中,用Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm)分离,流速1.0 mL/min;检测波长270 nm.结果表明,4种磺胺类药物在0.001～0.064 mg/L浓度范围内呈良好的线性关系,相关系数r为0.9997～0.9999;检出限为0.48～1.15 μg/L(S/N=3)；富集倍数在137～406之间；加标回收率为93.5％～104.0％.本方法操作简便、结果准确、灵敏度高.