摘要
采用全自动快速溶剂萃取法(ASE)将养殖场土壤中四环素、氯霉素、氟苯尼考、磺胺二甲基嘧啶、磺胺嘧啶和磺胺甲唑提取出来,建立液相色谱-三重四级杆串联质谱法定性、定量检测的分析方法。取畜禽养殖场土壤样品,风干后粉碎机粉碎,过60目筛网,准确称取15 g上述样品置全自动快速溶剂萃取池中,加20 g硅藻土,以甲醇与乙腈混合溶剂进行提取。提取完毕后,将提取液氮吹至近干,加1.0 mL甲醇溶解残渣,涡旋1 min后,用0.22μm滤膜过滤,上液相色谱-质谱仪定性、定量检测。四环素、氯霉素、氟苯尼考、磺胺二甲基嘧啶、磺胺嘧啶和磺胺甲唑在0.02~8.0μg/mL范围内线性关系良好,相关系数(r)均大于0.995;检测限分别为0.021、0.033、0.046、0.018、0.022和0.010μg/kg;平均回收率在83.9%~104.7%之间;重复性RSD分别为2.80%、3.17%、3.63%、2.27%、4.22%和3.93%(n=6)。实验方法具有快速、准确等特点,适用于养殖场土壤等样品的检测,为指导养殖户合理使用药物提供了技术依据。
An ASE method was developed for the determination of 6 antibiotics(tetracycline, chloramphenicol, florfenicol, sulfamethazine, sulfadiazine and sulfamethoxazole) residues in farm soil by using HPLC-MS/MS techniques.Farm soil samples were air-dried, curshed, and sieved by 60 mesh screen first.12.0 g crushed sample was submitted to solvent extraction tank with the addition of 20 g diatomite, then the mixture was extracted by methanol-acetontrile solution.The extracted solution was blown to nearly dry.The residue was dissolved by 1.0 mL methanol, volex for 1 min, filtered by 0.22 μm membrane, then qualitatively and quantitatively detected by HPLC-MS/MS.The detection of tetracycline, chloramphenicol, florfenicol, sulfamethazine, sulfadiazine, and sulfamethoxazole showed good linear relationships in the concentration ranges of 0.02~8.0 μg/mL,with correlation coefficients(r) all larger than 0.995.The detection limits for tetracycline, chloramphenicol, florfenicol, sulfamethazine, sulfadiazine and sulfamethoxazole were 0.021,0.033,0.046,0.018,0.022 and 0.010 μg/kg, respectively.The average recoveries were 83.9%~104.7%.The relative standard deviation(RSD) of repeatability were 2.80%,3.17%,3.63%,2.27%,4.22% and 3.93%(n=6).The experimental method was provn to be rapid and accurate, which is suitable for the detection of soil samples in farm and provided a technical basis for guiding the farmers to use drugs reasonably.
作者
毛娜
孙志洪
张丽
MAO Na;SUN Zhi-hong;ZHANG Li(Cang-zhou Research Institute of Ecological Environment Protection,Cangzhou 061000,China;Cangzhou Ecological Environment Monitoring Center of Hebei Province,Cangzhou 061000,China)
出处
《化学试剂》
CAS
北大核心
2021年第7期945-950,共6页
Chemical Reagents
