高效液相色谱法测定渔业水质中多西环素、四环素、土霉素、金霉素残留量

Determination of doxycycline,tetracycline,oxytetracycline,chlortetracycline residual amount in fishery water by high performance liquid chromatography(HPLC)

为了更好地监测渔业水质中四环素类抗生素药物残留，保护渔业环境，本研究建立了固相萃取一高效液相色谱检测渔业水质中多西环素、四环素、土霉素和金霉素4种四环素类抗生素的方法。经固相萃取柱纯化和富集，用甲醇洗脱。采用甲醇和咪唑缓冲液（pH7．2）作为流动相，7min内分离4种抗生素，外标法定量。标准曲线线性良好，以S／N=3计，多西环素、四环素、土霉素的检出限为0．01mg／L，金霉素的检出限为0．02mg／L，平均加标回收率为79．3％-98．7％，相对标准偏差（RSD）在3．91％-8．64％之间。本方法适用于渔业水质中多西环素、四环素、土霉素和金霉素抗生素的残留检测，可为渔业环境保护提供技术支持。

A high performance liquid chromatography method for the determination of doxycycline, tetracycline, oxy- tetracycline and chlortetracycline in fishery water was developed in order to protect the fishery environment. The sam- ples were purified and enriched with solid -phase extraction and eluted with methanol. The eluents were separated by the ODS - 3 column, with methanol and imidazole buffer （pH7.2） as mobile phase, followed by detection within 7 min. The linearity of standard curve was well by the external standard method. The detection limits （S/N = 3 ） of doxycycline, tetracycline, oxytetracycline were 0.01 mg/L and chlortetracycline was 0.02 mg/L, and the mean forti- fied recoveries ranged from 79.3% to 98.7%, with relative standard deviation in the region of 3.91% - 8.64%. This method was suitable for the detection of doxycycline, tetracycline, oxytetracycline and chlortetracycline residues in fishery water, which can provide technical support for fishery environment protection and aquatic products quality improvement.