基于部分碳化NH_(2)-MIL-101(Fe)的水中四环素类抗生素比色检测方法研究

A Colorimetric Method Based on Porous Carbon from NH_(2)-MIL-101(Fe)for Detection of Tetracyclines in Water

四环素类抗生素(Tetracyclines,TCs)在生产中的滥用会导致其在环境中的残留,极大提高了人体感染疾病的风险,并且目前仍缺乏快速、有效的检测手段。基于TCs在水中易与Fe^(2+)、Fe^(3+)产生强烈络合的特性,本文制备了一种部分碳化NH_(2)-MIL-101(Fe)用于水中TCs快速检测的比色检测方法。经惰性气氛煅烧法对NH_(2)-MIL-101(Fe)进行改性,制备了两种改性材料,并对两种改性材料和前体的表面形貌及化学结构进行了表征。对比了NH_(2)-MIL-101(Fe)和350、450℃下煅烧的改性材料与土霉素间的络合效果,实验结果表明,3种材料均可与土霉素络合,350℃煅烧得到的部分碳化材料具有最佳催化效果,并显示出良好的稳定性和分散性。在优化的检测条件下(催化剂投加量12μg·mL^(-1)、H_(2)O_(2)浓度6 mmol·L^(-1)、TMB浓度5 mmol·L^(-1)、pH=5.5、反应时间40 min),oxTMB在652 nm处的吸光度值与土霉素浓度之间呈现线性关系,线性范围为0.08~50μmol·L^(-1)(R^(2)=0.9822)。本文设计的比色方法可实现实际水体中TCs含量的灵敏、特异性检测,为完善水体安全监管体系提供了一定的理论与技术支撑。

The abuse of tetracyclines(TCs)in production had caused their residues in the environment,which induces undesirable effects on human health by increasing the risk of infection.At present,there is still a lack of rapid and effective detection methods.Because of the strong complexation of TCs with Fe 2+and Fe 3+in the aquatic environment,herein,a colorimetric detection method based on partially carbonized NH_(2)-MIL-101(Fe)was developed for detection of TCs in the aquatic environment:Inert atmosphere calcination was used to modify NH_(2)-MIL-101(Fe).Two modified materials were prepared,the surface morphology and chemical structure of those three materials were characterized.The complexations of NH_(2)-MIL-101(Fe)and two modified materials calcined at 350 and 450℃were compared with oxytetracycline.Experimental results showed that materials calcined at 350℃exhibited the best catalytic effect and showed good stability and dispersity.Under optimized conditions,the absorbance change of oxTMB at 652 nm had a linear relationship with oxytetracycline concentration,the linear range was 0.08~50μmol·L^(-1)(R ^(2)=0.9822).The designed colorimetric method could be applied to the quantification of TCs in practical water samples with high selectivity and sensitivity.It is of great significance for theoretical and technical support for improving the water safety supervision system.