摘要
从化学反应条件的控制及气相色谱一质谱（GC—Ms）和高效液相色谱／二极管阵列检测器（HPLC／DAD）联用方面，探讨了4-氨基偶氮苯的检测方法。实验表明，在样品中加入氢氧化钠，样品中的4-氨基偶氮苯和新鲜配制的连二亚硫酸钠发生反应，使4-氨基偶氮苯的碳碳双键断裂。释放的4-氨基偶氮苯在氯化钠存在的混合物中与叔丁基甲醚进行液液萃取。取叔丁基甲醚层进行分析，通过GC-Ms的保留时间及特征离子碎片并结合HPLC／DAl3紫外法对4一氨基偶氮苯进行定性和定量分析。4一氨基偶氮苯在2．5～30mg／kg范围内呈良好的线性关系，其线性方程为：y=91．23x＋5．272，相关系数，r=1．000，检出限为3．20mg／kg，平均回收率不低于90％。
A method for the determination of 4-aminoazobenzene was developed with two aspects of the control of chemical reaction conditions and the combination of GC - MS and HPLC/DAD. The results showed, in the presence of sodium hydroxide, 4-aminoazobenzene could react with fresh sodium dithionite solution, and broke the carbon - carbon double bond of 4-aminoazobenzene. The prepare time of sodium dithionite solution should be less than 3 hours to ensure its reductive. The product of 4-amino- azobenzene was extracted with t-butyl methyl ether in the presence of sodium chloride in 5 min. The analysis of 4-aminoazobenzene in organic layer of t-butyl methyl ether was carried out by GC - MS and HPLC/DAD method. A good linear relationship was obtained over the concentration of 4-aminoazobenzene in the range of 2. 5 -30 mg/kg. The linear equation was y =91.23x ＋5.272, with a corre- lation coefficient of 1. 000. The detection limit was 3.20 mg/kg, and the average recoveries were not less than 90% .
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第8期846-849,共4页
Journal of Instrumental Analysis
