有序介孔炭固相萃取-毛细管电泳联用测定水样中抗生素残留

建立了固相萃取-毛细管电泳联用测定河水水样中四环素类抗生素残留的分析方法.以有序介孔炭(OMC)作为固相萃取吸附剂,考察了有序介孔炭对四环素类抗生素(四环素、土霉素和多西环素)的吸附性能,探讨了影响固相萃取效率的因素,得到最佳萃取条件为:水样2.00 mL(pH 10.0),有序介孔炭5.0 mg,V(甲醇)∶V(乙腈)=1∶1的洗脱液4.00 mL,洗脱速度0.7 mL/min,此时富集倍数达50倍.在最佳的毛细管电泳分离条件下,各组分含量在3 000~11 000μg/L呈良好的线性关系,且各组分峰面积的日内相对标准偏差低于8.5%(n=5).四环素、土霉素和多西环素的最低检测限和平均回收率分别为1.96~2.14μg/mL和46.7%~93.6%.研究表明,有序介孔炭可作为环境样品中多西环素和土霉素的高效吸附材料.

Ordered mesoporous carbon-based solid phase extraction combined with capillary electrophoresis for the analysis of antibiotic tresidues in surface water

A solid-phase extraction （SPE）-capillary electrophoresis method tion of tetracyclines residues in surface water. It was aimed to evaluate the was developed for the determina- adsorption specificity of ordered mesoporous carbon （OMC） as solid phase extraction （SPE ） adsorbents with tetracychnes （tetracycline, oxy- tetracycline and doxycyctine） as model analytes. The parameters affecting the adsorption efficiency were inves- tigated in detail. The optimal extraction conditions were showed as follows： 2.00 mL water sample （ pH 10.0 ） , 5 mg OMC as adsorbent, 4.00 mL mixture of methanol and acetonitrile （ VMeOH ： VACN = 1 ： 1 ） as elu- ent at a speed of 13.7 mL · min^-1, enrichment factors of actual water sample were 50. Combined with optimal separation conditions of capillary electrophoresis, the linear range of the analytes varied from 3 000 to 11 000 μg · L^- 1, and relative standard deviations of peak area of each component were less than 8.5 % （ n = 5 ） in- tra-day analyses. The limits of detection and the average recovery （ for tetracycline, oxytetracycline and doxy- cycline） were in the range of 1.96 - 2.14 μg · mL^-1 and 46.7% - 93.6%, respectively. It demonstrated that OMC was a potential adsorbing material in preconeentrating doxyeyeline and oxytetraeycline from environ- mental samples.