固态顶空法测定苹果中的磷化氢残留  

Determination of phsophine residues in apples with solid headspace method

作　　者：李丽[1] 王跃进[1] 张凡华[1] 龚绍润[1] 刘彩虹[1] 詹国平[1] 刘涛[1] 

机构地区：[1]中国检验检疫科学研究院,北京100029

出　　处：《植物检疫》2014年第6期50-53,共4页Plant Quarantine

基　　金：2014年度国家质检总局动植物检疫处理专项;中国检科院基本科研业务费专项项目(2012JK029)

摘　　要：为开发水果中磷化氢残留的检测方法,本文采用固态顶空技术对苹果中的磷化氢进行了测定。顶空参数优化结果表明,60℃20 min平均回收率为101.1%,可确定为顶空处理条件。在此条件下使用气相色谱对一系列标准样品进行分析,得到磷化氢检测的线性范围为0.002 mg/kg^0.032 mg/kg,测定低限为0.002 mg/kg,远低于0.05 mg/kg的磷化氢残留限量要求。添加回收率结果表明,在0.002mg/kg^0.02 mg/kg范围的低、中、高3种加标水平的平均回收率为98.4%~104.1%,相对标准偏差为2.20%~2.63%。这些结果表明固态顶空法具有操作简便、灵敏度高、重现性好等优点。进一步的实际测定结果表明,熏蒸后苹果中的磷化氢残留在通风8 h后可降至安全水平。In order to determine phosphine residues in fruits, the solid headspace method was conducted for phosphine residues analysis in apples. Our results show that 101.1% recovery of phosphine residues could be achieved after 20 min heating at 60℃, and this optimized condition was used in further experiments. A series of phosphine standards were then determined with gas chromatography. The linear ranges of this method were determined to be 0.002 - 0.032 mg/kg, and the level of quantification （LOQ） was 0.002 mg/kg, which was far below the Maximum Residue Limits （0.05 mg/kg）. 1＆#215;, 5＆#215; and 10＆#215;LOQ ranging from 0.002 to 0.02 mg/kg phosphine were added in affix recovery tests. The average recoveries were ranging from 98.4% to 104.1% while the standard errors were ranging from 2.20% to 2.63%. These results indicated that the solid headspace method was simple, accurate and highly reproductive. Phosphine residues in fumigated apples were further determined. According to the results of actual samples, phosphine residues in apples would be acceptable after 8-h-aeration.

关 键 词：苹果 磷化氢残留 固态顶空法 

分 类 号：S481.8[农业科学—农药学] S661.1[农业科学—植物保护]