气相色谱-质谱法测定纺织材料及制品中16种限用有机锡类化合物  

Determination of 16 Restricted Organotin Compounds in Textile Materials and Their Products by GC-MS

作　　者：麦晓霞[1] 徐金梅 张子豪[1] 刘莹峰[1] 李全忠[1] 翟翠萍[1] 肖前[1] 郑建国[1] MAI Xiao- xia;XU Jin- mei;ZHANG Zi- hao;LIUJ Ying-feng;LI Quan- zhong;ZHAI Cui- ping;XIAO Qian;ZHENG Jian-guo(Guangdong Entry - Exit Inspection and Quarantine Bureau,Guangzhou 510623,China)

机构地区：[1]广东出入境检验检疫局,广东广州510623

出　　处：《分析测试学报》2018年第6期719-723,共5页Journal of Instrumental Analysis

基　　金：国家重点研发计划(2016YFF0203705)

摘　　要：采用气相色谱-质谱(GC-MS)技术建立了纺织材料及其制品中16种限用有机锡类化合物的测定方法。以甲醇和乙酸钠的混合溶液作为提取剂,对样品进行超声提取,提取液经四乙基硼酸钠衍生化后,再用正己烷进行萃取,DB-5MS(30 m×0.25 mm×0.25μm)色谱柱分离,气相色谱-质谱选择离子模式进行分析检测,内标法定量。16种有机锡类化合物在50~500μg/L质量浓度范围内与峰面积呈线性关系,方法的定量下限均为0.05 mg/L(0.15 mg/kg)。样品加标回收率为77.6%~106.0%,相对标准偏差(RSD,n=6)不大于8.3%。结果表明该方法快速可靠、准确简便,适用于纺织材料及制品中有机锡类化合物的分析检测。A gas chromatography-mass spectrometric（ GC-MS） method was developed for the determination of 16 organotin compounds in textile materials and their products. Samples were ultrasonically extracted with a mixture of methanol and sodium acetate,then the extract was derived with sodium tetraethyl borate,and extracted with n-hexane. The target ingredients were separated on a DB-5 MS（ 30 m × 0. 25 mm × 0. 25 μm） column. The 16 organotin compounds were analyzed in selective ion mode（ SIM）. Under the optimal conditions,the calibration curves for 16 organotin compounds were linear in the range of 50-500 μg/L,with limit of quantitation of 0. 05 mg/L（ 0. 15 mg/kg）.The recoveries ranged from 77. 6% to 106. 0%,with relative standard deviations（ RSDs,n = 6） not more than 8. 3%. This method was rapid,reliable,accurate and convenient to operate,and it was appropriate for the determination of organotin compounds in textile materials and their products in routine tests.

关 键 词：纺织品 有机锡 气相色谱-质谱 超声提取 

分 类 号：O657.63[理学—分析化学] S482.48[理学—化学]