快速溶剂萃取-气相色谱-质谱法测定涤纶纺织品中4-氨基偶氮苯  

GC-MS Determination of 4-Aminoazobenzene in Polyester Textiles with Separation by ASE

作　　者：沈俊杰 陈勇 潘建君 谈金辉 

机构地区：[1]湖州出入境检验检疫局,湖州313000

出　　处：《理化检验（化学分册）》2011年第8期935-936,941,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：涤纶纺织品中4-氨基偶氮苯用丙酮按快速溶剂萃取法(ASE)在120℃,10.34MPa条件下萃取分离,经蒸千后,加甲醇2.0mL溶解残渣,于此溶液中加入氢氧化钠溶液及连二亚硫酸钠溶液使之还原。在室温条件下用甲基叔丁基醚萃取,取其上清液,用HP-5MS毛细管柱进行色谱分离,并在离子源(70 eV,230℃)及质量扫描范围为35～350amu条件下进行质谱分析。4-氨基偶氮苯的质量浓度在1.0～150.0mg·L^(-1)范围内与峰面积呈线性关系。方法的测定下限(10S/N)为5.0mg·kg^(-1),方法的平均回收率为70.2%,相对标准偏差(n=6)均小于4.5%。4-Aminoazobenzene was separated from polyester textile sample by accelerated solvent extraction （ASE） with acetone under the condition of 120 ℃ and 10.34 MPa. The extract was evaporated to dryness at 35 ℃ and the residue was dissolved in 2. 0 mL of methanol. NaOH solution and sodium dithionite solution were added to reduce 4-aminobenzene. The solution was cooled to room temperature and extracted with methyl tert butyl ether. The supernatant was taken and used for GC-MS analysis, using HP-SMS capillary column for GC separation and El （70 eV, 230 ℃） with mass scanning range of 35--350 ainu in MS analysis. It was found that mass concentration of 4 aminoazobenzene in the range of 1. 0-150. 0 mg· L^-1 kept in linear relationship with values of corresponding peak area. Value of lower limit of determination （10S/N） was found to he 5.0mg· L^-1. Test for recovery was made by standard addition method, giving value of av. recovery of 70. 2%. Values of RSD＇s （n=6） found were less than 4.5%.

关 键 词：气相色谱-质谱法 快速溶剂萃取 涤纶纺织品 4-氨基偶氮苯 

分 类 号：O652.6[理学—分析化学]