摘要
建立了以多壁碳纳米管为固相萃取吸附剂分离富集牛奶、鸡蛋以及蜂蜜中的甲硝唑残留,并用高效液相色谱法测定的分析方法。考察了碳纳米管对甲硝唑的吸附效果,洗脱剂的种类及其用量、碳纳米管的长度及大小和上样速率对萃取率的影响,优化了固相萃取条件。在优化实验条件下,方法的线性范围为0.01~10mg,/L,检出限为0.25μg/kg;对3种实际样品分别进行1、10、50μg/kg3种水平下的加标回收实验,样品回收率为68%~112%,RSD为3.3%~17.1%,定量下限为0.8μg/kg。方法灵敏度高、简便快速且成本低,符合食品中低浓度兽药残留的分析方法要求。
A novel method for the determination of metronidazole (MNZ) in milk, egg and honey was established by using multi-wall carbon nanotubes (MWCNTs) as solid-phase extraction adsorbent combined with high-performance liquid chromatography (HPLC). The adsorptivity of MWCNTs for met- ronidazole was evaluated, and the effects of experimental conditions, including type and volume of the eluent, length and diameter of MWCNTs as well as flow rate on the extraction efficiency were investi- gated. Under the optimized SPE conditions, the calibration curve was linear in the range of 0.01 - 10 mg/L, and the limit of detection was 0. 25 μg/kg. The method was applied to detect the residues of metronidazole in milk, egg and honey. The spiked recoveries from the samples at three concentration levels of 1, 10 and 50 μg/kg were between 68% and 112% with RSDs of 3.3% - 17. 1% . The limit of quantification was 0. 8μg/kg, which is lower than that from the reference method of metronidazole in animal derived food. The results showed that multi-walled carbon nanotubes had good performance in the enrichment and purification. The proposed method had advantages of simplicity, sensitivity and low cost, and could meet the requirements for the determination of low MNZ residue in food.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第8期807-811,共5页
Journal of Instrumental Analysis
关键词
碳纳米管
固相萃取
甲硝唑
高效液相色谱法
carbon nanotubes
solid-phase extraction
metronidazole
high-performance liquid chromatography ( HPLC )