水产品中3种磺胺类药物和孔雀石绿的样品前处理及检测条件优化

Optimization of pretreatment and test conditions for the detection of 3 kinds of sulfonamides and malachite green in aquatic products

中文关键词:  水产品  磺胺类药物  孔雀石绿  高效液相色谱法  高效液相色谱-荧光法

英文关键词:aquatic products  sulfonamides  malachite green  high performance liquid chromatography  high performance liquid chromatography-fluorescence method

中文摘要:

      目的 优化样品前处理和检测条件对水产品中3种磺胺类药物和孔雀石绿进行定性、定量分析。 方法 分别参考农业部958号公告-12-2007和GB/T 20361-2006中的检测方法并作出相应的修改, 采用高效液相色谱法和高效液相色谱-荧光检测法检测水产样品中3种磺胺类药物和孔雀石绿的残留量。结果 测定3种磺胺类药物的最佳条件为: 以0.1%磷酸和乙腈(3:1,V:V)为流动相, 流速为0.8 mL/min, 3种磺胺类药物的回收率为79.5%~87.9%。测定孔雀石绿的最佳条件为: 以乙腈和乙酸铵(4:1, V:V)为流动相、流速为0.6 mL/min, 孔雀石绿的回收率为86.0%~86.9%。2种方法的相对标准偏差均小于10.0%。结论 2种检测方法具有样品前处理简单、回收率高、成本低、重复性较好等特点, 适用于批量水产品中3种磺胺类药和孔雀石绿残留量的测定。

英文摘要:

      Objective To optimize the sample pretreatment and test conditions for the qualitative and quantitative analysis of 3 kinds of sulfonamides and malachite green in aquatic products. Methods Refering to the test methods in ministry of agriculture notice No.958-12-2007 and GB/T 20361-2006 and making corresponding modifications respectively, 3 kinds of sulfonamides and malachite green residues in aquatic samples were detected by high performance liquid chromatography and high performance liquid chromatography-fluorescence method, respectively. Results The optimum conditions for the determination of respectively sulfonamides were 0.1% phosphoric acid and acetonitrile (3:1, V:V) as the mobile phase with the flow rate of 0.8 mL/min, and the recovery rates of respectively sulfonamides were 79.5%-87.9%. The optimum conditions for the determination of malachite green were acetonitrile and ammonium acetate (4:1, V:V) as mobile phases with the flow rate of 0.6 mL/min, and the recovery rates of malachite green were 86.0%-86.9%. The relative standard deviations of both methods were less than 10.0%. Conclusion The two methods are characterized by simple sample pretreatment, high recovery rate, low cost and good repeatability, and they are suitable for the determination of 3 sulfonamides and malachite green residues in batch aquatic products.