固相萃取气相色谱法测定水果中克菌丹和灭菌丹  

Determination of Captan and Folpet Pesticides Residues in Fruits by Solid Phase Extraction and Gas Chromatography

作　　者：于彦彬[1] 王淑菊[2] 谭培功 苗在京[1] 

机构地区：[1]农业部农产品质量安全监督检验测试中心青岛,青岛266109 [2]中国海洋大学,青岛266003 [3]青岛市环境监测中心站,青岛266003

出　　处：《分析化学》2008年第6期750-754,共5页Chinese Journal of Analytical Chemistry

摘　　要：采用硅镁吸附剂和硅胶作为混合固相萃取的净化方法,建立了固相萃取气相色谱法同时测定水果中克菌丹和灭菌丹的分析方法。研究了多种固相萃取柱和不同洗脱溶剂对克菌丹和灭菌丹保留行为的影响,优化了固相萃取净化方法及样品提取方法的分析条件。用GC-ECD检测,两种农药在0.05～2.0mg/L浓度范围内呈线性关系,相关系数大于0.997。苹果中4个浓度克菌丹和灭菌丹的加标回收率分别在100%～111%和104%～113%之间,RSD在3.0%～7.2%和2.8%～4.2%之间。在菠萝、草莓、梨和橙子中,克菌丹的平均回收率和RSD分别在95.6%～112%和2.5%～7.5%之间;灭菌丹在82.5%～96.4%和3.3%～8.0%之间,克菌丹和灭菌丹的方法检出限分别为0.012mg/kg和0.0056mg/kg。Determination of captan and folpet pesticides residues in fruits by gas chromatography are developed, and the silicon-magnesium sorbent and silica gel mixture were used as stuffing of solid phase extraction. The retention behavior of captan and folpet in different solid phase extraction cartridges and in various eluent solvent was studied. The optima/conditions for solid phase extraction clean up and sample extraction method are described. There was a good linear relationship within the range of concentration captan and folpet from 0. 05 to 2.00 mg/L by electron capture detection. The correlation coefficients for captan and folpet are more than 0.997. The samples was extracted by 50 mL acetonitrile after adding 15 mL H2O and 2.0 mL （ 1 ＋ 1 ） H3PO4. The extract in SPE column was eluted with dichloromethane： hexane： acetonitrile（49：50：1 ）. The recoveries of captan and folpet in apple for four level standard additions ranged from 100% - 113% with RSD of 2.8% -7.2%. The recoveries of captan were in the range of 95.6% -102% with RSD of 2.5% -7.5%, and folpet in the range of 82.5% -96.4% with RSD of 3.3% -8.0% for pine apple, strawberry, pear, orange. Method detection limit were 0. 012 mg/kg and 0. 0056 mg/kg for captan and folpet, respectively.

关 键 词：固相萃取 气相色谱法 克菌丹 灭菌丹 水果 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程]