Blackwell Paul A, Holten Lützhøft Hans-Christian, Ma Hai-Ping, Halling-Sørensen Bent, Boxall Alistair B A, Kay Paul
Cranfield Centre for EcoChemistry, Shardlow Hall, Shardlow, Derby, Derbyshire DE72 2GN, UK.
Talanta. 2004 Nov 15;64(4):1058-64. doi: 10.1016/j.talanta.2004.05.006.
A simple and rapid analytical method is presented in which the three veterinary antibiotics oxytetracycline (OTC), sulfachloropyridazine (SCP) and tylosin (TYL) are simultaneously extracted and determined in four different soils. Extractions were carried out by a combination of ultrasonic agitation and vortex mixing using a mixture of methanol, EDTA and McIlvaine buffer at pH 7 as the extractant solution. The extracts were then cleaned-up by a tandem solid phase extraction (SPE) method using an Isolute SAX anion exchange cartridge to remove natural organic matter and an Oasis HLB polymeric cartridge to retain the study compounds. Analysis was by HPLC-UV with additional fluorescence detection for SCP. Recoveries were in the range 68-85% for SCP in all soil types, 58-75% for OTC in sandy soils, 27-51% for OTC in clay containing soils, 74-105% for TYL and 47-61% in a clay soil. OTC and SCP were also extracted from liquid pig manure using a mixture of EDTA and McIlvaine buffer at pH 7 with ultrasonic agitation and vortex mixing with SPE clean-up and HPLC-UV analysis. Recoveries were greater than 77% and 58% for OTC and SCP, respectively. Limits of detection were 18mugkg(-1) for OTC and SCP and 40mugkg(-1) for TYL in soils and 70mugL(-1) for OTC and 140mugL(-1) for SCP in pig slurry.
本文介绍了一种简单快速的分析方法，可同时提取并测定四种不同土壤中的三种兽用抗生素，即土霉素（OTC）、磺胺氯哒嗪（SCP）和泰乐菌素（TYL）。采用甲醇、乙二胺四乙酸（EDTA）和pH 7的麦氏缓冲液混合溶液作为提取剂，通过超声搅拌和涡旋混合相结合的方式进行提取。然后，提取物通过串联固相萃取（SPE）方法进行净化，使用Isolute SAX阴离子交换柱去除天然有机物，使用Oasis HLB聚合物柱保留目标化合物。采用高效液相色谱-紫外检测法（HPLC-UV）进行分析，并对SCP进行额外的荧光检测。所有土壤类型中SCP的回收率在68-85%之间，砂质土壤中OTC的回收率为58-75%，含粘土土壤中OTC的回收率为27-51%，TYL的回收率为74-105%，粘土土壤中的回收率为47-61%。还使用pH 7的EDTA和麦氏缓冲液混合物，通过超声搅拌和涡旋混合，结合SPE净化和HPLC-UV分析，从液体猪粪中提取OTC和SCP。OTC和SCP的回收率分别大于77%和58%。土壤中OTC和SCP的检测限为18μg kg⁻¹，TYL的检测限为40μg kg⁻¹；猪粪浆中OTC的检测限为70μg L⁻¹，SCP的检测限为140μg L⁻¹。
