土壤及畜禽粪肥中四环素类抗生素固相萃取-高效液相色谱法的优化与初步应用

本研究优化了土壤和有机肥中3 种四环素类抗生素的提取和测定方法。方法经优化后，土壤和有机肥中的抗生素的提取效率达到52%~95%，且分析时间大大缩短。本研究还利用优化方法在天津进行了有机肥和菜地中3 种抗生素残留的初步调查。集约化养殖场的猪、鸡粪便中四环素类抗生素残留状况为: 金霉素（CTC）检出率达到78%，最高残留值达到563.8 mg/kg（干基）; 四环素（TC）和土霉素（OTC）检出率也高达56%，最高值分别达到34.8 mg/kg 和 22.7 mg/kg。在天津销售的几种商品有机肥中同样检测出四环素类抗生素的残留，残留水平与猪粪和鸡粪相当。菜田土壤样品中TCs的总检出率为64%，3.种抗生素中土霉素检出率最低为18%，最高值达到105.6 g/kg（风干基）; 四环素检出率为36%，最高值达到196.7 g/kg; 金霉素检出率为32%，最高值达到477.8 g/kg。在所调查土壤中，温室和大棚土壤TCs的残留水平高于露地土壤。占调查样品 27.3% 的菜田土壤中TCs总量超过欧盟规定的生态安全触发线（100 g/kg），存在一定的潜在生态风险。

Optimization of residual tetracyclines analysis in soils and manure using SPE-HPLC and pilot survey in Tianjin

Tetracyclines(TCs) are the most commonly detected antibiotics reminded in soils and manures in China. The survey of the residual status of tetracyclines is important for evaluating possible biological risks caused by direct exposure of bioorganisms and human beings. In this study, Analytical methods of three kinds of tetraclyinces, oxytetracycline, tetracycline and chlortetracycline, is optimized using SPE-HPLC. The residual status of TCs in soils and manure in Tianjin was investigated using the optimized method. The obtained method recovery rates for soils and manure are increased to the range of 52%-95%. In the surveyed feces samples from intensive piggeries and poultries, CTC is detected in 78% of manures with the highest mg/kg, and OTC and TC are detected in 56% of feces with the highest values of 34.8 and 22.7mg/kg, respectively. TCs are also detected in the market manure in Tianjin with similar residual levels and percentages to those in the feces samples. The total percentage of garden soils containing detectable TCs is 64% of the surveyed soils, and those for OTC, TC and CTC are 18%, 36% and 32%, respectively. The highest values for OTC, TC and CTC are 105.6, 196.7 and 477.8 g/kg in dry weight respectively. The residual levels in soils under facilities are higher than those in open fields. In 25% of surveyed garden soils, the total amounts of three kinds of TCs are higher than those in the trigger lines causing biological safety.