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固相萃取法与基质固相分散法在橙子中攀 p 有机磷农药残留分析中的应用菇
2013-03-19 16:13:17 益择发布p 有机磷农药残留分析中的应用菇
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； 杨海玉， 俞英， 郑秀丽：
l鬈《僦i≤“。d《⋯t⋯√。‰_。⋯㈣Ⅲ《##b#＆m。％㈣⋯。(。华南师范大学化学与环境学院，广东广州510006) 鎏 。#一一，， 、一⋯^#％女^碡w‰_⋯±‘⋯妇∞Ⅻ1％‰⋯m“自女㈤∞
摘要：建立了固相萃取(SPE)一反相高效液相色谱(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、c．。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％一102．7％，相对标准偏差(RSD)为0．9％
一4．9％。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：固相萃取；基质固相分散；高效液相色谱；有机磷农药；橙子
中图分类号：0658 文献标识码：A 文章编号：1000-8713(2008)06-0744一05 栏目类别：研究论文
；Application of solid—phase extraction and matrix solid—phase善
i dispersion in orange sample preparation for i
￡organophosphorous pesticide residues analy’sis 透
l舡 l蕊
爹YANG Haiyu，YU Ying，ZHENG Xiuli i
浚珏。o(School妒a塘鹏缸嘲and En魄懒懈强六South China Normal University，Guangzhou 510006，China) ∞震
Abstract：A solid—phase extraction(SPE)-reversed—phase high performance liquid chromatm
graphic(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(85：1 5，v／v)at the flow rate of 0．7 mL／min and
the ultraviolet wavelength of 254 nnl．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斗g／L，respectively．The average recoveries ranged from 87．3％to 102．7％with the relative
standard deviations of 0．9％一4．9％at the spiking levels of 0．10 and 0．5 mg／kg in orange sam—
pies．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：solid—phase extraction(SPE)；matrix solid—phase dispersion(MSPD)
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