| 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 |
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| 引用本文： | 唐春玲,张文清,夏玮,左萍萍,朱恩.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[J].中国土壤与肥料,2011(2):92-95. |
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| 作者姓名： | 唐春玲 张文清 夏玮 左萍萍 朱恩 |
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| 作者单位： | 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 |
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| 基金项目： | 上海市科学技术委员会资助项目 |
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| 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。
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| 关 键 词： | 固相萃取 高效液相色谱 四环素类 有机肥 |
Determination of tetracycline antibiotic residues in organic manure by SPE-HPLC |
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| TANG Chun-ling,ZHANG Wen-qing,XIA Wei,ZUO Ping-ping,ZHU En.Determination of tetracycline antibiotic residues in organic manure by SPE-HPLC[J].Soil and Fertilizer Sciences in China,2011(2):92-95. |
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| Authors: | TANG Chun-ling ZHANG Wen-qing XIA Wei ZUO Ping-ping ZHU En |
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| Institution: | 1.Shanghai Key of Functional Materials Chemistry,East China University of Science and Technology,Shanghai 200237;2.Shanghai Agricultural Technology Extension and Service Center,Shanghai 201103) |
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| Abstract: | 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. |
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| Keywords: | solid-phase extraction(SPE) HPLC tetracyclines organic manure |
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