多次顶空-捕集阱捕集/气相色谱质谱联用分析皮革中的挥发性有机物

Determination of volatile organic compounds in leather by multiple headspace-trapping and gas chromatography/mass spectrometry

建立了多次顶空-捕集阱捕集/气相色谱质谱联用-基质加标校正曲线测定皮革中的挥发性有机物的方法。在10 m L无挥发性有机物的试剂水中加入1g皮革样品和2 g NaCl,顶空时间30 min,温度80℃,捕集阱加压循环3次。气质联用法分析皮革中的挥发性有机物,采用DB-624（60 m×0.25 mm×1.4μm）的色谱柱分离挥发性有机物,并采用基质加标校正标准曲线对目标化合物进行定量。目标化合物在1~400μg/L或20~400μg/L的内线性关系良好,R在0.995~0.999之间,不同浓度的加标回收率在80.8%~125%之间,相对标准偏差在1.3%~16%之间,检出限在0.08~21.7μg/kg。

The method was established to determine the volatile organic compounds（ VOCs） in leather by multiple headspace-trapping with gas chromatography/mass spectrometry（ GC/MS） and the spiked matrix calibration curve. In the headspace method,1g leather sample and 2g sodium chloride were added into10 m Lwater without volatile organic compounds. The headspace time was 20 minutes,the headspace temperature was 80℃,and the trap pressured cycles was three times. The gas chromatography/mass spectrometry（ GC/MS）was used for the analysis of the VOCs in the leather. The DB-624 fused silica capillary column（ 60 m,0. 25 mm i. d.,1. 4μm film thickness） was selected for chromatographicseparation of the VOCs. The spiked matrix calibration curve was used for the quantification of the target compounds. The target compounds exhibited a good linearity in 1 ~ 400μg/L or 20 ~ 400μg/L,with the correlation coefficients of 0. 995 ~ 0. 999. The average recovery of the spike sampleswith different concentrationswas 80. 8% ~ 125%,and the RSDs of the spike samples was 1. 3% ~ 16%. The detection limit of the VOCs was 0. 08 ~ 21. 7μg/kg.