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

作　　者：沈浩 林丽娜 程洁 林观基 吴淑曼 刘俊 朱振瓯 Shen Hao;Lin Lina;Cheng Jie;Lin Guanji;Wu Shuman;Liu Jun;Zhu Zhenou(Bureau Veritas Consumer Products Services Shenou(Wenzhou)Co.,Ltd.,Wenzhou 325006,China;Comprehensive Technical Service Center of Wenzhou Customs,Wenzhou 325027,China;Wenzhou Sheng Tai Environmental Technology Co.,Ltd,Wenzhou 325024,China)

机构地区：[1]必维申瓯质量技术服务温州有限公司,浙江温州325006 [2]温州海关综合技术服务中心,浙江温州325027 [3]温州市升泰环境科技有限公司,浙江温州325024

出　　处：《化学分析计量》2021年第4期42-44,49,共4页Chemical Analysis And Meterage

摘　　要：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.

关 键 词：皮革 短链氯化石蜡 气相色谱-负化学离子源质谱法 

分 类 号：O657[理学—分析化学]