色谱

色谱

• 研究论文 • 上一篇    下一篇

固相萃取法与基质固相分散法在橙子中有机磷农药残留分析中的应用

杨海玉,俞英,郑秀丽   

  1. School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China
  • 收稿日期:2008-07-18 修回日期:2008-09-18 出版日期:2008-11-30 发布日期:1983-06-25
  • 通讯作者: 俞英
  • 基金资助:

Application of solid-phase extraction and matrix solid-phase dispersion in orange sample preparation for organophosphorous pesticide residues analysis

YANG Haiyu, YU Ying, ZHENG Xiuli   

  1. School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China
  • Received:2008-07-18 Revised:2008-09-18 Online:2008-11-30 Published:1983-06-25
  • Contact: YU Ying

PDF

787

摘要： 建立了固相萃取(SPE)-反相高效液相色谱(RP-HPLC)同时测定橙子中痕量辛硫磷、二嗪农有机磷农药残留量的方法。样品经甲醇超声提取、C18固相萃取柱净化后,采用液相色谱柱分离，以乙腈-水(体积比为85∶15)为流动相等度洗脱，于254 nm下紫外检测。结果表明:在0.1～10.0 mg/L和0.4～10.0 mg/L范围内,辛硫磷、二嗪农的质量浓度与峰面积呈良好的线性关系；样品的加标平均回收率为87.3%～102.7%，相对标准偏差(RSD)为0.9%～4.9%。将该分析结果与用基质固相分散法(MSPD)处理样品所得的结果相比较，发现SPE对二嗪农的提取效果较好，而MSPD对辛硫磷的提取效果较好，但两种方法都能较好地净化样品，均能满足残留量的分析要求。

关键词: 橙子 , 高效液相色谱, 固相萃取, 基质固相分散, 有机磷农药

Abstract: A solid-phase extraction (SPE)-reversed-phase high performance liquid chromatographic (RP-HPLC) method for the determination of phoxim and diazinon in oranges has been developed. The analytical procedure involved in the ultrasonic extraction with methanol, the purification using a C18 SPE column, and the separation on a liquid chromatography column by the isocratic elution with acetonitrile-water (85∶15, v/v) at the flow rate of 0.7 mL/min and the ultraviolet wavelength of 254 nm. The results demonstrated that the linear ranges of phoxim and diazinon were 0.1-10.0 mg/L and 0.4-10.0 mg/L, and the detection limits of 4.1 and 6.7 μg/L, respectively. The average recoveries ranged from 87.3% to 102.7% with the relative standard deviations of 0.9%-4.9% at the spiking levels of 0.10 and 0.5 mg/kg in orange samples. The analytical results obtained by SPE were compared with those of the matrix solid-phase dispersion (MSPD) cleanup method. The recovery of diazinon using the SPE cleanup method was better, but the MSPD cleanup method was much suitable for phoxim. The lower background can be obtained via each cleanup method.

Key words: high performance liquid chromatography (HPLC), matrix solid-phase dispersion (MSPD), oranges , organophosphorous pesticides, solid-phase extraction (SPE)