色谱

色谱

• 研究论文 • 上一篇    下一篇

基质固相分散-高效液相色谱法测定鲫鱼肌肉中残留的辛硫磷

刘茜, 刘晓宇*, 邱朝坤, 王小宝, 任红敏   

  1. College of Food Science and Technology, Huazhong Agricultural University, Wuhan 430070, China
  • 收稿日期:2009-02-10 修回日期:2009-04-10 出版日期:2009-07-30 发布日期:1982-06-25
  • 通讯作者: 刘晓宇

Application of matrix solid-phase dispersion for the determination of phoxim in crucian carp samples by high performance liquid chromatography

LIU Qian, LIU Xiaoyu*, QIU Chaokun, WANG Xiaobao, REN Hongmin   

  1. College of Food Science and Technology, Huazhong Agricultural University, Wuhan 430070, China
  • Received:2009-02-10 Revised:2009-04-10 Online:2009-07-30 Published:1982-06-25
  • Contact: LIU Xiaoyu

PDF

653

被引次数

36

摘要： 建立了鲫鱼肌肉中残留的辛硫磷的基质固相分散-高效液相色谱-二极管阵列检测(MSPD-HPLC-DAD)的分析方法。通过优化样品处理条件,确定选取0.50 g鲫鱼肌肉样品与1.5 g弗罗里硅土、0.5 g无水硫酸钠混合研磨,并采用丙酮-正己烷溶液(体积比为40:60)为洗脱剂,洗脱剂用量为25 mL。优选的最佳色谱条件为：ODS色谱柱(250 mm×4.6 mm,5 μm),流动相为甲醇-水(体积比为50:50),流速0.6 mL/min,检测波长270 nm,进样量为20 μL。在上述条件下,辛硫磷质量浓度在0.01～10 mg/L范围内与响应信号呈良好的线性关系(r20.9994),检出限为3.3 μg/kg;相对标准偏差为1.1%～6.3%(n7);3个添加水平(0.05,0.1,1 mg/kg)下得到的回收率为88%～112%。该方法操作简单,耗时少,精密度高,符合农残分析的要求。

关键词: 残留, 高效液相色谱, 基质固相分散, 鲫鱼 , 农药, 辛硫磷

Abstract: An analytical method was developed for the determination of phoxim residue in the muscle of crucian carp, which involved matrix solid-phase dispersion (MSPD) followed by high performance liquid chromatography (HPLC) with diode array detector. Under optimal conditions, 0.5 g tissue sample was dispersed with 1.5 g Florisil and 0.5 g anhydrous sodium sulphate, transferred to a cartridge. The cartridge was eluted with 25 mL acetone-hexane (40:60, v/v). The phoxim was separated on an ODS column (250 mm×4.6 mm, 5 μm) with methanol-water (50:50, v/v) as the mobile phase at the flow rate of 0.6 mL/min, then detected by a diode array detector at 270 nm. The injection volume was 20 μL. The linear range of the method was 0.01~10 mg/L and the detection limit was 3.3 μg/kg. The average recoveries spiked at the levels of 0.05, 0.1, 1 mg/kg ranged from 88% to 112% with the relative standard deviations (RSDs) of 1.1% ~6.3%. The method is quick, simple and can meet the requirement of the analysis of pesticide residues.

Key words: crucian carp , high performance liquid chromatography (HPLC), pesticide, phoxim, residue, matrix solid-phase dispersion (MSPD)