气相色谱-负化学离子源质谱法测定皮革中短链氯化石蜡

Determination of short chain chlorinated paraffins in leather by gas chromatography-negative chemical ionization mass spectrometry

建立了气相色谱–负化学离子源–质谱法测定皮革中短链氯化石蜡的检测方法。样品经正己烷超声提取,浓硫酸净化后,采用气相色谱–负化学离子源–质谱仪测定,以外标法定量。短链氯化石蜡的质量浓度在2.5~50 μg/mL范围内具有良好的线性关系,相关系数均大于0.997 1,检出限为10 mg/kg,定量限为30 mg/kg。在50、100、200 mg/kg加标水平下,样品平均回收率为80.4%~110.4%,测定结果的相对标准偏差为3.8%~9.5%(n=6)。该方法灵敏、简单、准确,可用于皮革制品中短链氯化石蜡的测定。

A method for the determination of short chain chlorinated paraffins in leather by gas chromatography negative chemical source mass spectrometry(GC-NCI-MS)was established.After ultrasonic extraction with n-hexane and purification with concentrated sulfuric acid,the samples were determined by gas chromatography negative chemical source mass spectrometry and quantified by external standard method.There was a good linear relationship between the mass concentration of short chain chlorinated paraffins and the chromatographic peak area in the range of 2.5-50 μg/mL,the correlation coefficients were more than 0.9971.The detection limit was 10 mg/kg and the quantification limit was 30 mg/kg.At the spiked levels of 50,100 and 200 mg/kg,the average recoveries were 80.4%-110.4%,and the relative standard deviations were 3.8%-9.5%(n=6).The method is sensitive,simple and accurate,and it can be used for the determination of short chain chlorinated paraffins in leather products.