有机肥中4类典型兽药抗生素的多残留测定

生态与农村环境学报 ›› 2012, Vol. 28 ›› Issue (5): 587-594.doi:

有机肥中4类典型兽药抗生素的多残留测定

葛峰,郭坤,谭丽超,戴亦军

环境保护部南京环境科学研究所

收稿日期:2012-03-30 修回日期:2012-04-23 出版日期:2012-09-25 发布日期:2012-10-08
作者简介:葛峰（1981-），男，江苏扬中人，副研究员，博士生，主要研究方向为有毒有害化学品的环境影响。E-mail:gefeng@nies.org
基金资助:
环保公益性行业科研专项(200809092)

Simultaneous Determination of Residues of Four Typical Categories of Veterinary Antibiotics in Organic Fertilizers

GE Feng, GUO Kun, TAN Li-Chao, DAI Yi-Jun

Nanjing Institute of Environmental Sciences,Ministry of Environmental Protection

Received:2012-03-30 Revised:2012-04-23 Online:2012-09-25 Published:2012-10-08

摘要/Abstract

摘要： 建立了固相萃取-超高效液相色谱-串联质谱（SPE-UPLC-MS/MS）法同时测定有机肥中7种磺胺类、4种氟喹诺酮类、4种四环素类和3种大环内酯类抗生素残留的方法。采用乙腈和磷酸盐缓冲液（pH＝3）的混合液作为有机肥样品的提取溶液，用强阴离子交换柱（SAX）亲水亲脂平衡萃取柱（HLB）串联进行提取液的富集和纯化。以甲醇-φ＝0.1%的甲酸溶液作为流动相，进行液相质谱分析。18种抗生素在5～500 μg·kg^-1的浓度范围内线性关系良好，决定系数（r^２）≥0.99。以3倍信噪比估算磺胺类、氟喹诺酮类、四环素类和大环内酯类的检测限分别为0.37～4.65、0.43～2.42、0.94～2.78和0.83～4.20 μg·kg^-1，这4类抗生素50和500 μg·kg^-12个添加水平的样品平均加标回收率分别为71.6%～94.3%、72.3%～86.7%、71.0%～102.2%和70.7%～93.3%，相对标准偏差在2.1%～11.4%之间。采用所建方法对南京地区市售8种有机肥中18种抗生素含量的测定结果显示，除磺胺类外，其他抗生素均有不同程度的检出。

关键词: SPE-UPLC-MS/MS, 有机肥, 兽药残留

Abstract: A new method using SPE-UPLC-MS/MS was developed to determine residues of four typical categories of veterinary antibiotics in organic manure. The method uses the solution composed of acetonitrile and phosphate buffer (pH=3) for extraction of organic manure samples, and the series of SAX and HLB to purify and enrich the extract. Methanol-φ=0.1% formic acid was chosen as carrier for liquid chromatographic analysis. When the concentrations of the 18 antibiotics were in the range of 5-500µg•kg^-1, they showed good linear relationships, with determination coefficients (r²) ≥ 0.99. When the mass concentration of the antibiotics was raised to the range of 50-500µg•kg^-1, the recovery rates of sulfonamides, fluoroquinolones, tetracyclines and macrolides varied in the range from 71.6% to 94.3%, from 72.3% to 86.7%, from 71.0% to 102.2% and from 70.7% to 93.3%, respectively, with relative standard deviation varying in the range of from 2.1% to 11.4%. This method was applied to determine residues of veterinary antibiotics in organic fertilizers on sale in Nanjing. In addition to sulfonamides, others were also detected to a varying extent.

Key words: SPE-UPLC-MS/MS, organic fertilizers, veterinary drug residue

中图分类号:

X830
O657.63

葛峰, 郭坤, 谭丽超, 戴亦军. 有机肥中4类典型兽药抗生素的多残留测定[J]. 生态与农村环境学报, 2012, 28(5): 587-594.

GE Feng, GUO Kun, TAN Li-Chao, DAI Yi-Jun. Simultaneous Determination of Residues of Four Typical Categories of Veterinary Antibiotics in Organic Fertilizers[J]. Journal of Ecology and Rural Environment, 2012, 28(5): 587-594.

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