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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。
Nine halogenated hydrocarbon compounds in leather were determined by headspace gas chromatography-mass spectrometry. Leather samples (1.000 g, debris, size no more than 0.5 cm x 0.5 cm, thickness 1 mm) were placed in a headspace bottle and equilibrated at 110 ° C for 45 min with an injection volume of 1 mL and separated on a GS-Gaspro capillary column using Program temperature, from 80 ℃ ~ 250 ℃. Mass spectrometry determination with EI ion source (230 ° C), in the range of 35 ~ 350amu full scan mass and external standard method. There is a linear relationship between the quality of 9 kinds of halogenated hydrocarbon compounds and their corresponding detection signals, and the correlation coefficients of all linear regression equations are all greater than 0.995. The method of determination of the lower limit (10S / N) between 1 ~ 2mg.kg-1. The leather sample was taken as the base, and the standard addition method was used to make the recovery test. The recoveries were between 82.5% and 106%. The relative standard deviations (n = 6) of the measured values ranged from 2.4% to 6.2%.