氯苯胍在鸡粪中的残留及降解动态分析

Residue and Degradation Dynamics Analysis of Robenidine in Chicken Manure

为揭示不同环境下鸡粪中氯苯胍的残留降解规律,模拟不同环境状态,研究氯苯胍在不同起始浓度、温度和pH下的降解特征。鸡粪中氯苯胍经乙腈提取,正己烷除脂,分散固相萃取法进行净化,以C 18色谱柱进行分离,高效液相色谱二极管阵列检测器进行检测。结果表明,氯苯胍在0.1~30μg/g浓度间呈线性相关,相关系数R 2为0.9996,检测限为0.03μg/g,定量限为0.10μg/g;鸡粪中氯苯胍在0.10、0.50、1.00μg/g 3个添加水平下,外标法定量,回收率在83.81%~94.61%之间,批内相对标准偏差为2.74%~8.93%,批间相对标准偏差为7.62%~9.72%;鸡粪中氯苯胍降解速率受起始浓度、温度和pH影响,药物起始浓度越高,鸡粪中氯苯胍降解速率越慢,当药物起始浓度为10、40、200μg/g时,在30 d内,氯苯胍降解速率分别为100%、100%和77.10%,半衰期分别为2.36 d、8.61 d和15.43 d;鸡粪中氯苯胍降解速率随温度升高而加快,当温度为4℃时,氯苯胍在30 d后降解速率为43.30%,而在25℃和45℃时完全降解;酸化或碱化后氯苯胍降解速率较未处理组明显加快,在试验期内均降解完全。因此,在进行粪便无害化处理时,可通过提高堆肥温度、将堆体酸化或碱化以提高氯苯胍降解速率,进而降低环境污染风险。

To reveal the residual degradation pattern of robenidine in chicken manure under different environments,in this paper,effects of different environmental conditions(concentrations,temperature and pH)on the degradation of robenidine were investigated.The robenidine in chicken manure was extracted by acetonitrile.After degreasing by n-hexane,manure samples were cleaned up by dispersive solid phase extraction.Target analyte was separated by a C 18 column and detected by high performance liquid chromatography with diode array detector.Robenidine showed a linear correlation between 0.1μg/g and 30μg/g with a correlation coefficient of 0.9996.The detection limit was 0.03μg/g and the quantification limit was 0.10μg/g.The recoveries ranged from 83.81%to 94.61%with intra-batch coefficients of variations of 2.74%to 8.93%and inter-batch coefficients of variations of 7.62%to 9.72%for the quantification of robenidine in chicken manure at three spiked levels of 0.10μg/g,0.50μg/gand 1.00μg/g.The degradation rate of robenidine in chicken manure was affected by the starting concentration,temperature and pH:the higher the starting concentration of the drug,the slower the degradation rate of robenidine in chicken manure was.When the starting concentration of the drug was 10μg/g,40μg/g and 200μg/g,the degradation rates of robenidine in chicken manure were 100%,100%and 77.10%within 30 days,with half-lives of 2.36 days,8.61 days and 15.43 days,respectively.The degradation rate of robenidine in chicken manure was accelerated with the increase of temperature.When the temperature was 4℃,the degradation rate of robenidine was 43.30%after 30 days,while it was completely degraded at 25℃and 45℃.The degradation rate of robenidine was significantly accelerated after acidification and alkalinization compared with the untreated group,and all of them were completely degraded during the test period.In the harmless disposal of manure,the degradation rate of robenidine could be increased by increasing the composting temperature and acidifying or alkalizing the compost,thus reducing the risk of environmental contamination.