固相微萃取-气相色谱法测定橙汁中残留有机氯杀虫剂
GC Determination of Organochlorine Insecticides in Orange Juice with Solid Phase Microextraction
摘 要
自制碳纳米管涂层萃取探头,顶空固相微萃取-气相色谱法测定橙汁中有机氯杀虫剂六六六和滴滴涕,优化了影响萃取效率的因素:萃取时间和温度、离子强度、有机溶剂、顶空体积、pH和样品的稀释度等.在0.05~6.0 μg·L-1范围内呈线性关系,方法的检出限在0.003~0.022 μg·L-1之间.该方法用于橙汁样品的测定,对不同的杀虫剂,加标回收率为71.0%~131.0%,相对标准偏差小于10%.
顶空固相微萃取
气相色谱法
有机氯杀虫剂
橙汁
Nanocarbon tube
Headspace-solid phase microextraction
Gas chromatography
Organochlorine insecticides
Orange juice
Abstract
A new extraction probe prepared by coating nanocarbon tube on stainless steel wire was used in the solid-phase microextraction (SPME) of organochlorine insecticides which were determined by GC with electron-capture detection. In the GC-analysis,SPME was integrated with the head-space technique (HS-SPME). Various factors influential to the HS-SPME,i.e. time and temperature of extraction,ionic strength,kind of organic solvents,volume of headspace,pH value of the sample solution and its dilution,etc.,were studied and optimized. Eight insecticides were determined with ranges of linearity within 0.05-6.0 μg·L-1,and detection limits (S/N=3) ranged from 0.003-0.022 μg·L-1. Using orange juice sample as matrix,tests for recovery and precision were made by addition of standard solutions of the insecticides,giving values of recovery in the range 71.0%-131.0%,and RSD′s (n=6) less than 10%.
中图分类号 O657.37
所属栏目 工作简报
基金项目
收稿日期 2008/2/17
修改稿日期
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备注田孟魁(1964-),男,河南伊川人,副教授,研究方向为色谱分析.
引用该论文: TIAN Meng-kui,FENG Xi-lan. GC Determination of Organochlorine Insecticides in Orange Juice with Solid Phase Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(9): 833～836
田孟魁,冯喜兰. 固相微萃取-气相色谱法测定橙汁中残留有机氯杀虫剂[J]. 理化检验－化学分册, 2008, 44(9): 833～836
被引情况:
【1】叶存玲,刘清玲,谢国红,王治科, "分散液相微萃取-高效液相色谱法测定水样中扑虱灵和哒螨灵",理化检验－化学分册 47, 1391-1394(2011)
【2】林海禄,彭雪娇,闫红1, "离子液体液相微萃取-气相色谱法测定水果中3种有机磷农药残留",理化检验－化学分册 47, 1440-1442(2011)
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参考文献
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【2】Chong S L,Wang D X,Hayes J D,et al. Sol-gel coating technology for the preparation of solid phase microextraction fibers of enhanced thermal stability[J]. Anal Chem,1997,69:3889．
【3】Liu M M,Zeng Z R,Fang H F. Preparation and application of the sol-gel-derived acrylate/silicone co-polymer coatings for headspace solid-phase microextraction of 2-chloroethyl ethyl sulfide in soil[J]. J Chromatogra A,2005,1076:16．
【4】Liu M M,Liu Y,Zeng Z R,et al. Preparation and characteristics of high Ph-resistant sol-gel alumina-based hybrid organic-inorganic coating for solid-phase microextraction of polar compounds[J]. J Chromatogra A,2006,1108:149．
【5】Li X J,Zeng Z R,Gao S Z,et al. Preparation and characteristics of sol-gel-coated calixarene fiber for solid-phase microextraction[J]. J Chromatogra A,2004,1023:15．
【6】Cai L S,Zhao Y Y,Gong S L,et al. Use of a novel sol-gel dibenzo-18-crown-6 solid-phase microextraction fiber and a new derivatizing reagent for determination of aliphatic amines in lake water and human urine[J]. Chromatographia,2003,58(9/10):615．
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【8】王树涛,尤宏,王炎.固相微萃取活性炭涂层萃取头对水中有机物的定性分析[J].理化检验-化学分册,2006,42(10):785．
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【10】Zhao R S,Wang X,Fu S,et al. A novel headspace solid-phase microextraction method for the exact determination of organochlorine pesticides in environmental soil samples[J]. Anal Bioanal Chem,2006,384:1584．
【11】Dong C Z,Zeng Z R,Yang M. Determination of organochlorine pesticides and their derivations in water after HS-SPME using polymethylphenylvinylsiloxane-coated fiber by GC-ECD[J]. Water Research,2005,39:4204．
【12】Rodrigues M V N,Reyes F G R,Rehder V L G,et al. An SPME-GC-MS method for determination of organochlorine pesticide residues in medicinal plant infusions[J]. Chromatographia,2005,61:291．
【13】Dong C Z,Zeng Z R,Li X J. Determination of organochlorine pesticides and their metabolites in radish after headspace solid-phase microextraction using calixarene fiber[J]. Talanta,2005,66:721．
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