食品科学 ›› 2011, Vol. 32 ›› Issue (14): 206-209.doi: 10.7506/spkx1002-6630-201114043

• 分析检测 • 上一篇    下一篇

多壁碳纳米管基质固相分散-高效液相色谱测定牛奶中6种四环素

王学翠,刘 冰,张璐鑫,季晶晶,施金秋,张 航,杨宗惠,吴 宏*   

  1. 徐州师范大学化学化工学院,江苏省功能材料绿色合成重点实验室
  • 出版日期:2011-07-25 发布日期:2011-06-18
  • 基金资助:
    国家质量技术监督检验检疫总局项目(2009IK131);江苏省自然科学基金项目(BK2008121); 徐州市科技计划项目(XM08C026)

Determination of 6 Tetracycline Antibiotics in Milk by Matrix Solid-Phase Dispersion Extraction Using Multiwalled Carbon Nanotubes Coupled with HPLC

WANG Xue-cui,LIU Bing,ZHANG Lu-xin,JI Jing-jing,SHI Jin-qiu,ZHANG Hang,YANG Zong-hui,WU Hong*   

  1. (Jiangsu Key Laboratory of Green Synthetic Chemistry for Functional Materials, School of Chemistry and Chemical Engineering, Xuzhou Normal University, Xuzhou 221116, China)
  • Online:2011-07-25 Published:2011-06-18

摘要: 以多壁碳纳米管为吸附材料,建立基质固相分散萃取高效液相色谱法测定牛奶中6种四环素。将多壁碳纳米管、EDTA、草酸和样品研磨混匀装柱,经含甲酸的甲醇洗脱后HPLC多波长紫外检测。6种四环素的检出限0.01~0.03μg/mL,回收率78.7%~105.2%,相对标准偏差小于12%。多壁碳纳米管基质固相分散萃取牛奶中四环素的回收率优于C18,可推广到食品等复杂样品中其他农兽药多残留分析。

关键词: 高效液相色谱法, 四环素, 基质固相分散, 碳纳米管

Abstract: A matrix solid-phase dispersion extraction (MSPDE) method was developed to extract 6 tetracycline antibiotics (TCs) from milk samples using multiwalled carbon nanotubes (MWCNTs) as adsorbent prior to high performance liquid chromatography (HPLC) determination. Milk samples, MWCNTs, oxalic acid, and EDTA were evenly ground and then packed into a glass syringe as dispersion column. The analytes were eluted with methanol containing formic acid, and detected by HPLC with variable wavelength detector at 365 nm. The limits of detection (LODs) for 6 TCs ranged from 0.01 to 0.03μg/mL. Their recoveries in spiked milk samples were in the range of 78.7%-105.2% with relative standard deviations of less than 12%. #br# MSPD exhibited higher recovery in extracting 6 TCs as compared to C18 column extraction, suggesting that the developed MSPD procedure can be applied for the multiresidues analysis of pesticides and veterinary drugs in foods.

Key words: tetracycline antibiotics, matrix solid-phase dispersion extraction, carbon nanotubes, high performance liquid chromatography

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