文献类型：期刊文献

中文题名：固相萃取-高效液相色谱法测定有机肥中四环素类抗生素药物残留

英文题名：Determination of tetracycline antibiotic residues in organic manure by SPE-HPLC

作者：唐春玲[1];张文清[1];夏玮[1];左萍萍[1];朱恩[2]

机构：[1]上海市功能性材料化学重点实验室华东理工大学,上海200237;[2]上海农业技术推广中心,上海201103

年份：2011

期号：2

起止页码：92

中文期刊名：中国土壤与肥料

外文期刊名：Soil and Fertilizer Sciences in China

收录：CSTPCD;;北大核心:【北大核心2008】；CSCD:【CSCD_E2011_2012】；

基金：上海市科学技术委员会资助项目(073919109)

语种：中文

中文关键词：固相萃取;高效液相色谱;四环素类;有机肥

外文关键词：solid-phase extraction（SPE）; HPLC; tetracyclines; organic manure

摘要：建立了固相萃取-高效液相色谱(SPE-HPLC)法测定有机肥中土霉素(OTC)、四环素(TC)和金霉素(CTC)3种四环素类抗生素残留的方法。肥料样品采用甲醇、EDTA和McIlvaine缓冲液的混合液(pH=7.2)为提取液,用强阴离子交换柱(SAX)-亲水亲脂萃取柱(HLB)串联进行纯化和富集。采用甲醇-乙腈-0.01mol/L草酸溶液为流动相,进行HPLC分析。3种抗生素的线性范围为0.10～20 mg/L,OTC、TC和CTC的检测限分别为0.03、0.03和0.05 mg/L。不同添加水平的样品加标回收率为64%～86%,RSD在4.14%～8.16%之间。该方法测定了上海市场上40种肥料,发现部分样品有四环素类抗生素的残留物。
A method using solid-phase extraction（SPE）combined with high-performance liquid chromatography（HPLC）has been developed for simultaneous determination of three kinds of tetracycline antibiotic（oxytetracycline,OTC,tetracycline,TC and chlortetracycline,CTC）residues in organic manure.The samples were extracted with a mixture of methanol,EDTA and McIlvaine buffer at pH=7.2.The extracts were then cleaned-up and enriched by a tandem SPE method using an Isolute SAX anion exchange cartridge and an Oasis HLB polymeric cartridge.Analysis was performanced by HPLC and the mobile phase was methanol-acetonitrile-0.01 mol/L oxalic acid solution.The calibration curve was linear in the range 0.1～20 mg/L.The limit of detection（LOD）was 0.03 mg/L,0.03 mg/L,0.05 mg/L and the recovery rates were 64%～86% with RSD ranging from 4.14% to 8.16% for OTC,TC,CTC in organic manure.With the method,40 kinds of manures from Shanghai market were detected and the results showed that some samples contained tetracycline antibiotic residues.