摘要
利用1-己基-3-甲基咪唑六氟磷酸盐离子液体萃取-高效液相色谱法检测养殖场周边地表水中四环素类抗生素的含量。样品前处理比较了锰、铜、锌和钴金属离子与抗生素配合后的离子液体萃取效果。在流动相中比较草酸、柠檬酸、磷酸二氢钾、三氟乙酸作为流动相添加剂对四环素类抗生素峰型的改善效果。结果表明,锰离子作为金属配合剂,萃取效率更高,以磷酸二氢钾作为流动相添加剂,基线噪声较小,检测限最低,3种抗生素峰型较好。方法的线性范围为0.05~8.0 mg/L,具有良好的线性关系(0.999 4~1.000 0),较低的检出限(3.5~8.4×10^-3 mg/L)及较好的精密度RSD(0.31%~0.68%)。实际样品重复检测3次的方法回收率为86.4%~103%,相对标准偏差≤2.10%。
A method was developed for the determination of tetracycline antibiotics in surface water neighboring livestock farm by high performance liquid chromatography with ionic liquid(1-hexyl-3-methylimidazolium hexafluorophosphate) as extraction.In order to obtain better extraction efficiency,four kinds metal ions(Mn^2+,Cu^2+,Zn^2+ and Co^2+) as tetracycline antibiotics complexant were added to the samples during sample pretreatment respectively.The extraction efficiency with Mn^2+ as the complexing agent was higher than the others.Furthermore,the effects of oxalic acid,citric acid,potassium dihydrogen phosphate and trifluoroacetic acid as mobile phase additives on the peak shape improvement of tetracycline antibiotics were investigated.It was better for baseline,noise and detection limit when the mobile phase was added potassium dihydrogen phosphate.The correlation coefficient of proposed method was more than 0.999 4 in the range of 0.05~8.0 mg/L.The limits of detection were ranged from 3.5~8.4×10^-3 mg/L and RSDs for peak area were 0.31%~0.68%.The recovery rate of real sample was 86.4% to 103% and the RSDs were less than 2.10% for peak area(n=3).
作者
周晚晴
黄金飞
金小玲
李键
卢浈乐
叶明立
陈梅兰
ZHOU Wanqing;HUANG Jin-fei;JIN Xiao-ling;LI Jian;LU Zhen-le;YE Ming-li;CHEN Mei-lan(College of Biology and Environmental Engineering,Zhejiang Shuren University,Hangzhou 310015,China;Zhejiang Furniture and Hard-ware Research Institute,Hangzhou 310013,China)
出处
《化学试剂》
CAS
北大核心
2020年第2期180-185,共6页
Chemical Reagents
基金
浙江省自然科学基金资助项目(LY20B070007)
浙江省质量技术监督系统科研计划项目(20180114)。
