分散固相萃取-气相色谱法测定水果中的六六六农药残留研究.pdfVIP

安徽农业科学，Journal of Anhui Agri. Sci.2015 ,43(5) :199-2∞，243 责任编辑乔利利责任校对李岩 分散固相萃取-气相色谱法测定水果中的六六六农药残留研究 未然，朱雅丽，牛俊莉 (新疆林业科学院，新疆乌鲁木齐 83州) 摘要 [目的]建立采用多壁碳纳米管(MWCNTs) 和乙二膝-N- 丙基硅炕(PSA) 为吸附剂的分散回相萃取(dSPE) 净化、气相色谱测定水 果中六六六残留量的方法。[方法]水果样JL 用乙蜻提取，再加入 NaCI 和元水 MgSO，液液分离，然后在样品提取液中加入元水 MgSO，、 四A 和多壁碳纳米管进行分散团相净化。[结果]所测定的4 种六六六的质量浓度在O. ∞5 -0.2∞ mglL 范围内与其峰面积比呈线性关 系，相关系数(R) 均大于0.9988 ，方法对所测定的9 种物质的检出限均小于1.(削 mglL，样品加标回收率为 809毛 -110% ，相对标准偏 差(n =6) 为2.42% -5.999毛。[结论]该方法有较好的灵敏度，能够满足样品测定的要求。 关键词 分散固相萃取;六六六;多壁碳纳米管 中图分类号 S481 + • 8 文献标识码 A 文章编号 0517 -6611(2015)05 -199 -02 Determination of Hexachlorocyclohexanes in Fruits by Dispersive Solid Phase Extraction and Gas Chromat句p-aphy ZHUR却1 ， ZHU Ya-旨，NIU Jun-li (Xinjiang Academy of Forestry ,Urumqi ,Xinjiang 83αX泊) Abstract [ Objective] A simple method for the determination of 4 Hexachlorocyclohexanes in fruits employing modified dispersive solid phase extraction (d-SPE) followed by gas chromatography-tan-dem ECD (GC-ECD) analysis was developed. [Method] For the fresh fruit samples ,the pesticides were extracted by acetonitrile or acetonitrile ,respectively , and then liquid-liquid partitioning formed by adding a址lydrOUS MgSO. and NaCl; followed by a simple cleanup step using multi-walled carbon nanotubes (MWCNTs) and PSA for samples extraction 描 dispersive solid phase extractio叫d-SPE) . The pesticide was confirmed and determined by g画 chromatography w他 ECD detector. [Result] The linear range were O. ∞15 -0.2∞ mglL( R ;;;.0. 998 8). The recoveries for all the pesticides studied were from 80% to 110% with relative standard deviation (RSD) from 2.429毛 to 5.999岛. [ Conclusion] The results showed that the method was simple and quick. It was suitalole for the determination of 4 Hexachlorocyclohexanes in fruits. Key words Dispersive solid phase extraction; BHC; MWCNT