微流控芯片联用高效液相色谱-荧光检测器同时测定肉类食品中4种磺胺类药物残留

Simultaneous determination of 4 kinds of sulfonamides residues in meat products by microfluidic chip and high performance liquid chromatography-fluorescence detector

中文关键词:  微流控芯片  高效液相色谱-荧光检测器  磺胺类药物  肉类食品

英文关键词:microfluidic chip  high performance liquid chromatography-fluorescence detector  sulfonamides  meat products

中文摘要:

      目的 建立一种使用微流控芯片进行肉类食品前处理, 并结合高效液相色谱-荧光检测器(high performance liquid chromatography-fluorescence detector, HPLC-FLD)同时测定肉类食品中4种磺胺残留的方法。方法 样品先用乙酸乙酯提取后, 在微流控芯片中用2 mol/L盐酸溶液反萃取和正己烷脱脂, 收集盐酸流出液100 μL, 与0.5 g/mL醋酸钠溶液按照1:1 (V:V)混合, 加入0.2 g/L荧光胺50 μL进行衍生化反应, 采用岛津ODS-3色谱柱进行分离, 流动相为乙腈-2%乙酸水溶液。结果 4种磺胺完全分离且在0.01~1.00 mg/L呈良好的线性关系, 在50、100、200 μg/kg 3个添加水平下, 平均回收率为72.1%~91.6%, 相对标准偏差为4.7%~13.6%, 方法检出限为1~5 μg/kg。结论 该方法具有快速、方便、经济、除脂效果好、环保等优点, 适合肉类食品中4种磺胺类药物残留分析, 并且提供了一个新的样品前处理思路。

英文摘要:

      Objective To develop a method for simultaneous determination of 4 kinds of sulfonamides residues in meat products by microfluidic chip and high performance liquid chromatography-fluorescence detector (HPLC-FLD). Methods The sample was extracted with ethyl acetate, and then reextracted with 2 mol/L hydrochloric acid solution in the microfluidic chip and degreased with n-hexane. Then 100 μL of hydrochloric acid effluent was collected and mixed with 0.5 g/mL sodium acetate solution at 1:1 (V:V), the derivations were performed by adding 0.2 g/L fluorescent amine 50 μL, Shimadzu ODS-3 chromatographic column was used for separation, and the mobile phase was acetonitrile-2% acetic acid aqueous solution. Results Four kinds of sulfonamides were completely separated and showed a linear relationship at 0.01?1.00 mg/L. The recoveries were 72.1%?91.6% at 50, 100 and 200 μg/kg levels, the relative standard deviations were 4.7%?13.6%, and the limits of detection were 1?5 μg/kg. Conclusion This method is rapid, convenient, economical, good in degreasing effect and environmental protection, which is suitable for the analysis of 4 kinds of sulfonamides residues in meat products and provides a new idea for sample pretreatment.