土壤和堆肥中四环素类抗生素的检测方法优化及其在土壤中的降解研究  

Method optimization for determination of tetracyclines in soils and compost and their degradation in soils

作　　者：李玲玲[1] 黄利东[1] 霍嘉恒[2] 锺仁赐[2] 章永松[1] 

机构地区：[1]教育部环境修复与生态健康重点实验室,浙江省亚热带土壤与植物营养重点实验室,浙江大学环境与资源学院,浙江杭州310029 [2]台湾大学农业化学研究所,台湾台北10617

出　　处：《植物营养与肥料学报》2010年第5期1176-1182,共7页Journal of Plant Nutrition and Fertilizers

基　　金：浙江省重大科技专项(2008C12061-1);科技部农业科技成果转化资金项目(2010GB23600669);国家科技支撑计划(2008BADA6B02)资助

摘　　要：在对土霉素(OTC)、四环素(TC)和金霉素(CTC)3种四环素类抗生素的高效液相色谱(HPLC)检测分析方法以及在土壤和堆肥中的提取方法进行改进和优化的基础上,采用该方法进行了3种抗生素在土壤中的降解试验。结果表明,选用Agilent Eclipse XDB-C8(4.6×150 mm,5μm)色谱柱,以0.01 mol/L草酸/乙腈/甲醇(79/10.5/10.5,v/v/v)为流动相,紫外检测波长268 nm,流速1.0 mL/min,进样量5μL,采用外标法定量,可使3种四环素类抗生素在20 min内全部洗脱并达到基线分离;在0～10 mg/L范围内,抗生素浓度与峰面积呈显著的线性关系,相关系数(r)均>0.999。土壤和堆肥样品中的OTC、TC和CTC可用1 mol/L NaCl/0.5 mol/L草酸/乙醇(25/25/50,v/v/v)混合溶液提取,其回收率在76.0%～92.5%之间。加入到土壤中的抗生素在25℃下避光培养49 d后,在壤土和红土中的降解率分别是67%～72%和36%～46%,对应的半衰期分别为26～30 d和46～75 d,说明抗生素在壤土中比红土中容易降解。此外,3种抗生素在壤土中的半衰期没有显著性差异,而在红土中CTC和TC的降解速率显著高于OTC。Based on method improvement and optimization for determination of Oxytetracycline（OTC）,Tetracycline（TC） and Chlortetracycline（CTC） using high-performance liquid chromatography（HPLC） and the extraction method of tetracyclines（TCs） in soils and compost,the degradation of these three TCs in soils was studied.The results indicated that these three TCs could be completely eluted to baseline separation in 20 min by a column of Agilent Eclipse XDB-C8（4.6×150 mm,5 μm）.The mobile phase was 0.01 mol/L oxalic acid-ACN-MeOH（79/10.5/10.5,v/v/v） at a flow rate of 1.0 mL/min.The injection volume of sample solution was 5 μL and the UV detector wavelength was at 268 nm.A significant linear correlation between these TCs under the concentration of 0-10 mg/L was observed（r 0.999）.The TCs in soils and compost could be extracted by a mixture solution of 1 mol/L NaCl/0.5 mol/L oxalic acid/ ethanol（25/25/50,v/v/v）,with the recoveries ranged from 76.0% to 92.5%.After 49 d of incubation at 25 oC in the dark condition,the degradation rates of the TCs in loam soil and red clay were 67%-72% and 36%-46%,respectively.The corresponding half-life of TCs was 26-30 d in loam soil and 46-75 d in red clay,respectively,indicating that the degradation of TCs in the loam soil was significantly faster than that in the red clay.Moreover,there was no significant difference between the half-life of TCs in the loam soil,while the degradation rates of CTC and TC in the red clay were significantly higher than that of OTC.

关 键 词：四环素类 抗生素 土壤 堆肥 检测 降解 

分 类 号：S141.4[农业科学—肥料学] S153[农业科学—农业基础科学]