四环素类抗生素残留的HPLC-CL联用新方法研究

发布时间：2018-07-29 13:06

【摘要】：目的:我国作为抗生素的生产大国,四环素类抗生素药物的滥用、不合理应用现象比较普遍。由此造成的细菌耐药、畜产品药物残留、过敏中毒反应等危害日益明显,已直接威胁到人类的健康与安全。本文旨在建立可同时测定四环素(TC)、土霉素(OTC)、金霉素(CTC)和甲烯土霉素(MTC)四种类抗生素残留的HPLC-CL检测新方法,并对其在食品安全中的应用进行研究。方法:在最优的反应条件下用HPLC-CL联用法测定四环素类抗生素。待测的四环素类样品通过手动进样器进入高效液相系统,流动相为3.5×10-3mol/L甲烷磺酸(CH4O3S)的乙腈-水(20:80,v:v)溶液,流速为0.85ml/min,柱温30℃,检测波长270nm,在C18分离柱上进行等度洗脱分离,经UV检测器分离定性。柱后流出液首先与MCLA溶液混合,接着与Ce(Ⅳ)溶液混合。最后在化学发光检测仪的流通池中产生化学发光信号,由光电倍增管将其转换成电信号,并由工作电脑记录发光信号强度。结果:四环素(TC)、土霉素(OTC)、金霉素(CTC)和甲烯土霉素(MTC)检出限分别为2.5×10-9 mol/L,4.1×10-9 mol/L,1.0×10-8 mol/L,4.5×10-9 mol/L,它们的相对标准偏差为3.54%-8.76%(n=7)。经实际样品检测,得出猪肉的回收率为84.85%-111.0%,RSD为3.85%-10.87%,牛奶的加标回收率为76.49%-115.7%,RSD为4.17%-10.70%。结论:本文建立了一个快速测定食品中四环素类抗生素残留的HPLC-CL新方法。与其他体系相比,洗脱方式简单,简化了流动相;与HPLC-UV相比,提高了选择性,解决柱后流出物的干扰问题;与HPLC-MS/MS相比,降低了检测成本;最后,明确了发光机理,为化学发光技术的发展提供了理论依据。通过实际样品检测,表明该方法在实际检测中操作简便、分析快速,选择性好、灵敏度高、回收率高,具有十分广阔的应用前景。
[Abstract]:Objective: as a large country producing antibiotics, the abuse of tetracycline antibiotics is common. Bacterial resistance, drug residues in animal products, allergic poisoning and other hazards are becoming more and more obvious, which have directly threatened the health and safety of human beings. A new HPLC-CL method for simultaneous determination of tetracycline (TC), oxytetracycline (OTC), chlortetracycline (CTC) and methylene oxytetracycline (MTC) was established and its application in food safety was studied. Methods: tetracycline antibiotics were determined by HPLC-CL under optimal reaction conditions. The tetracycline samples to be tested entered the high performance liquid phase system through a manual sampler. The mobile phase was a 3.5 脳 10-3mol/L methane sulfonic acid (CH4O3S) acetonitrile-water (20: 80 v: v) solution with a flow rate of 0.85 ml / min, column temperature of 30 鈩，

本文编号：2152763