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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
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麦晓霞,徐金梅,张子豪,刘莹峰,李全忠,翟翠萍,肖前,郑建国 广东出入境检验检疫局 
基金项目:国家重点研发计划(2016YFF0203705)
中文摘要: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×0.25 μm)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50~500 μg/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。
中文关键词:纺织品  有机锡  气相色谱-质谱  超声提取
 
Determination of 16 Restricted Organotin Compounds in Textile Materials and Their Products by GC-MS
Abstract: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-5MS(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.
Key Words:textile  organotin  gas chromatography-mass spectrometry(GC-MS)  ultrasonic extraction
引用本文:麦晓霞,徐金梅,张子豪,刘莹峰,李全忠,翟翠萍,肖前,郑建国.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[J].分析测试学报,2018,37(6):719-723.
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