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 insoils and compost and their degradation in soils
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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（4.6150 mm，5 m）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 5 L，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 2630 d 和 4675 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。Abstract: Based on method improvement and optimization for determination of Oxytetracycline (OTC), Tetracycline (TC) and Chlortetracycline (CTC) using highperformance 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 (4.6150 mm, 5 m). The mobile phase was 0.01 mol/L oxalic acidACNMeOH (79/10.5/10.5, v/v/v) at a flow rate of 10 mL/min. The injection volume of sample solution was 5 L 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 halflife 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 halflife 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.
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Keywords:
- tetracyclines /
- antibiotics /
- soil /
- compost /
- HPLC /
- determination
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期刊类型引用(9)
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