蔬菜中8种有机氯农药前处理方法的比较
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摘要
目的通过测定蔬菜中8种有机氯农药,比较固相萃取净化与浓硫酸净化两种前处理方法。方法试样经固相萃取净化与浓硫酸净化两种方法处理,分别用正己烷、石油醚溶解残渣,采用Rtx-1701色谱柱进行分离,ECD检测器检测,以保留时间定性,以峰面积定量。结果以浓硫酸净化测定蔬菜中的有机氯农药含量,3种浓度的加标回收率在81.5%～101.3%之间,精密度RSD在1.6%～3.7%之间。以固相萃取净化,其回收率在59.7%～101.2%之间,精密度在2.1%～4.5%之间。结论浓硫酸净化的回收率远优于固相萃取法,故采用浓硫酸净化法测定蔬菜中的8种有机氯农药。
Objective To determine eight organochlorine pesticides in vegetables, two pretreatment methods, solid phase extraction(SPE) and concentrated sulfuric acid(CS) were compared.Methods The sample was treated by solid phase extraction and concentrated sulfuric acid. The residue was dissolved by n-hexane and petroleum ether, separated by Rtx-1701 chromatographic column and detected by ECD detector. The retention time was qualitative and the peak area was quantitative.Results The content of organochlorine pesticides in vegetables was determined by concentrated sulfuric acid purification. The recoveries of the three concentrations ranged from 81.5% to 101.5%, and the precision RSD ranged from 1.6% to 3.7%. The recovery rate of solid phase extraction purification ranged from 59.7% to 101.2%, and the precision RSD ranged from 2.1% to 4.5%. Conclusion The recovery of concentrated sulfuric acid is much better than that of solid phase extraction. The method of concentrated sulfuric acid purification is used to determine 8 organochlorine pesticides in vegetables.
Objective To determine eight organochlorine pesticides in vegetables, two pretreatment methods, solid phase extraction(SPE) and concentrated sulfuric acid(CS) were compared.Methods The sample was treated by solid phase extraction and concentrated sulfuric acid. The residue was dissolved by n-hexane and petroleum ether, separated by Rtx-1701 chromatographic column and detected by ECD detector. The retention time was qualitative and the peak area was quantitative.Results The content of organochlorine pesticides in vegetables was determined by concentrated sulfuric acid purification. The recoveries of the three concentrations ranged from 81.5% to 101.5%, and the precision RSD ranged from 1.6% to 3.7%. The recovery rate of solid phase extraction purification ranged from 59.7% to 101.2%, and the precision RSD ranged from 2.1% to 4.5%. Conclusion The recovery of concentrated sulfuric acid is much better than that of solid phase extraction. The method of concentrated sulfuric acid purification is used to determine 8 organochlorine pesticides in vegetables.
引文
[1] 李杰,韦桂欢,席骁,等.固相萃取—气相色谱法测定水中有机氯农药[J].舰船科学技术,2010,12(32):107-110.
[2] 田芹,吴淑琪,佟玲,等.中国典型类型土壤中有机氯农药和多氯联苯成分分析标准物质的研制[J].岩矿测试,2015,34(2):238-244.
[3] 魏进,张盈,陈湘燕,等.不同产地黄芪中有机氯农药残留的分析[J].实验研究,2015,32(10):110.
[2] 田芹,吴淑琪,佟玲,等.中国典型类型土壤中有机氯农药和多氯联苯成分分析标准物质的研制[J].岩矿测试,2015,34(2):238-244.
[3] 魏进,张盈,陈湘燕,等.不同产地黄芪中有机氯农药残留的分析[J].实验研究,2015,32(10):110.