鱼塘沉积物中氯霉素的超声萃取、净化与测定

Extraction and Determination of Chloramphenicol in Sediment of Aquaculture Pond

通过对鱼塘沉积物中氯霉素的提取、净化洗脱和测定方法研究,尝试了以甲醇为萃取剂,利用超声萃取鱼塘沉积物中的氯霉素,然后再以层析柱净化,甲醇作洗脱液洗脱,用高效液相色谱法(HPLC)分析氯霉素含量。结果表明,当用甲醇超声萃取3次(30、10和10min),并用甲醇作层析柱净化洗脱液时,提取效果比较理想。利用HPLC分析氯霉素含量的色谱条件为:HpersilODS色谱柱4.6mm×250mm,进样量10μL,流速1.0mL·min-1,柱温30℃,检测波长275nm,流动相为乙腈:水=60:40(V/V)。此方法的检测限为7μg·kg-1,平均回收率为82.74%～88.38%,精密度RSD为0.4%～3.3%。应用该方法检测得到食用鱼塘和金鱼鱼塘沉积物中氯霉素的残留量分别为0.1716和0.1224mg·kg-1。

A procedure for determination of chloramphenicol （CAP） in aquaculture pond sediment was developed. Ultrasonic was employed to extract CAP from samples. The conditions were studied including extraction solvents, time, clean-up methods and analytical conditions of HPLC. The results showed that the optimal conditions for obtaining CAP from pond sediment were as follows： ultrasonic extracting 30 min and 10 min twice with methanol, cleaning up from sediment with methanol using solid column, detecting by HPLC at 275 nm, with acetonitrile/ water （60/40, V/V） as mobile phase at a flow rate of 1.0 mL ·min^-1, with an injection volume of 10 μL, at column temperature of 30 ℃. This technique is able to detect chloramphenicol residues at the level of 7 μg·kg^-1, and the overall recoveries were 82.74%-88.38% with R S D values 0.4%-3.3%. With the technique, the CAP residue concentration from the sediment in pounds of goldfish and edible fish were 0.171 6 mg·kg^-1 and 0.122 4 mg·kg^-1 respectively.