摘要
用顶空气相色谱-质谱联用法测定了皮革中9种卤代烃化合物。皮革样品(1.000g,碎片,大小不超过0.5cm×0.5cm,厚度1mm)置于顶空瓶中,于110℃平衡45min,进样量为1mL,用GS-Gaspro毛细管色谱柱进行分离,采用程序升温,从80℃～250℃。质谱测定中用EI离子源(230℃),在35～350amu质量范围内全扫描方式并用外标法定量。9种卤代烃化合物的质量与其相应检测信号值之间呈线性关系,各线性回归方程的相关系数均大于0.995。方法的测定下限(10S/N)在1～2mg.kg-1之间。以皮革样品为基体,用标准加入法做回收试验,测得回收率在82.5%～106%之间,测定值的相对标准偏差(n=6)在2.4%～6.2%之间。
Head-space gas chromatography in hyphenation with mass spectrometry was used in the determination of 9 volatile halogen substituted hydrocarbons（VXH′s）.Sample of leather（1.000 g,in slices with dimensions of 0.5 cm ×0.5 cm×1 mm） was equilibrated in a head-space bottle at 110 ℃ for 45 min,and 1 mL of sample was introduced into the instrument for analysis.GS-Gaspro capillary column was used in the separation with programed temperature elevation from 80 ℃ to 250 ℃.In MS determinations,EI（230 ℃）,whole scanning mode（35-350 amu） and external standard method were adopted.Linear relationships between values of response signals and masses of the 9 VXH′s were obtained in definite ranges with values of correlation coefficients of their linear regression equations larger than 0.995.Values of lower limits of determination（10S/N） were found in the range of 1-2 mg·kg-1.Tests for recovery were made by standard addition method on the base of leather samples,values of recovery found were ranged from 82.5% to 106%,with values of RSD′s（n=6） ranged from 2.4% to 6.2%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2011年第12期1395-1397,1401,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家质检总局科技计划项目(2010IK039)
