花生中丁酰肼残留测定的两种衍生方法比较  

Comparison of 2 Derivatization Methods in GC-MS Determination of Residual Butyryl Hydrazide in Peanuts

作　　者：宓捷波[1] 王云凤[1] 秦洪建[1] 

机构地区：[1]天津出入境检验检疫局,天津300456

出　　处：《理化检验（化学分册）》2009年第4期442-445,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：对气相色谱-质谱联用法（GC-MS）测定花生中残留丁酰肼含量时，衍生化所用的两种衍生试剂，水杨醛和2-硝基苯甲醛，在衍生反应的介质及条件、检测响应值、标准曲线的线性范围以及测定下限和回收率等方面作了详细比较。试验结果表明：两种试剂均适合作为衍生试剂，但从衍生反应操作简便以及较高的灵敏度和较好的回收率等方面考虑，用水杨醛作衍生试剂效果更好，而且在衍生化过程中用离心法除去反应而残留的水杨醛更保证了检测的精密度。应用这一方法所测得丁酰肼的测定下限（10S／N）为0．005mg·kg^-1，用标准加入法测得的回收率在98．0％～99．4％之间，测定值的相对标准偏差（n-6）在1．5％～3．6％之间。Methods of derivatization, in GC-MS determination of residual butyryl hydrazide in peanuts, with salicyl aldehyde and with 2-nitrobenzaldehyde as derivatizing reagents were compared with respect to the reaction medium and condition of derivatization, response values, range of linearity of standard curves, and values of lower limit of determination as well as the recovery. It was found that both of the reagents were feasible to be used in the derivatization under the optimum condition, but salicyl aldehyde was preferred due to its easy operation of derivatization reaction, higher sensitivity and better recovery. Removal of the un-reacted salicyl aldehyde by centrifugation was the guarantee for precision of measurements. Lower limit of determination （10S/N） of the method using salicyl aldehyde as derivatizing reagent was found to be 0. 005 mg·kg^-1 of butyryl hydrazide, and the values of recovery obtained were in the range of 98. 0%--99.4%, and the values of RSD＇s （n=6） were in the range of 1.5%-31 6%.

关 键 词：气相色谱-质谱联用法 衍生化试剂 水杨醛 2-硝基苯甲醛 丁酰肼 花生 

分 类 号：O657.63[理学—分析化学]