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(1.000 g,碎片,大小不超过0.5 cm×0.5 cm,厚度1 mm)置于顶空瓶中,于110 ℃平衡45 min,进样量为1 mL,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35~350 amu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1~2 mg·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%.