摘要
建立了一种同时测定水产品中甲砜霉素和氟甲砜霉素药物残留的超高效液相色谱（UPLC）方法。样品经乙酸乙酯提取,正己烷液-液分配除脂,过HLB固相萃取小柱,用3mL10%甲醇淋洗,5mL100%甲醇洗脱,洗脱液用氮气吹干,残渣用1mL10%乙腈水溶液定容。采用超高效液相色谱分离,二极管阵列检测器检测,外标法定量。甲砜霉素在0.05~2.0mg/L,氟甲砜霉素在0.025~1.0mg/L范围线性关系良好,相关系数分别为0.9996、0.9999;样品加标平均回收率分别为80.0%、95.8%;相对标准偏差分别为5.6%、11.2%,甲砜霉素、氟甲砜霉素检出限分别为10μg/kg、5μg/kg。
An ultra performance liquid chromatographic method （UPLC） has been developed for the determination of thiamphenicol and florfenicol residues in aquatic products. The samples were extracted with ethyl acetate, cleaned up by n-hexane liquid-liquid extraction, and then purified by HLB SPE column. After washing with 3 mL 10% methanol, the residues were eluted from the cartridge with 5 mL methanol. The eluate was evaporated to dryness under nitrogen stream, and then dissolved in 1 mL 10% acetonitrile. The residues were determined by ultra performance liquid chromatography with photodiode array detection and quantified by external standard method. The linear ranges were 0.05 - 2.0 mg/L for thiamphenicol and 0. 025 - 1.0 mg/L for florfenicol. The detection limit were 10 μg/kg for thiamphenicol and 5 μg/kg for florfenicol. The average recoveries in spiked sample were 80.0% - 95.8%.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2008年第4期525-528,共4页
Chinese Journal of Analytical Chemistry
关键词
甲砜霉素
氟甲砜霉素
水产品
残留分析
超高效液相色谱
Thiamphenicol, florfenicol, aquatic products, residue, ultra performance liquid chromatography
