蚕丝制品中辛基酚和壬基酚残留量的气相色谱-质谱法测定  

Determination of octylphenol and nonlyphenol in silk products by gas chromatography-mass spectrometry

作　　者：李淳[1] 邱思聪 任忠海[1] 梁文杰[2] 余林[3] 曹维强[2,3] 林家奎 

机构地区：[1]广东出入境检验检疫局,广东广州510623 [2]惠州出入境检验检疫局,广东惠州516006 [3]广东工业大学轻工化工学院,广东广州510006 [4]广东省丝绸纺织集团有限公司,广东广州510004

出　　处：《纺织学报》2014年第5期91-96,共6页Journal of Textile Research

基　　金：广东省科技计划项目(2012B020305004)

摘　　要：通过固相萃取气相色谱-质谱法，建立了同时测定蚕丝制品中辛基酚和壬基酚的分析方法，对提取溶剂的选择、提取方式、固相萃取条件以及气相色谱和质谱条件进行了研究。结果表明：蚕丝样品以正己烷作为萃取溶剂，经超声萃取，石墨化炭黑柱（Supelclean Envi—Carb）净化，辛基酚和壬基酚的定量离子质核比均为107，定性离子质核比分别为206和220，在优化实验条件下，这种方法的定量下限为0．1mg／kg，样品加标回收率分别为86．20％～106．20％和81．10％～91．80％，相对标准偏差分别为7．81％和4．56％（0．1mg／kg，n=6）。气相色谱一质谱检测方法操作简捷，灵敏度高，可满足国际贸易过程中对蚕丝制品中辛基酚、壬基酚的测定要求。A method was developed for measurement of octylphenol（OP） and nonylphenol（NP） residues in textile prodocts by gas chromatography-mass spectrometry, the choice of extraction solvent, extracting methods, solid phase extraction conditions and conditions of gas chromatography-mass spectrometry were studied. The study showed that the OP and NP in silk samples were detected by n-hexane solvent with ultrasonic-assisted extraction, purified by Supelclean Envi-Carb solid phase extraction column and determined by gas chromatography-mass spectrometry. Quantitative ions were selected at m/z of 107 for OP and NP, and qualitative ions were selected at m/z of 206 for OP and m/z 220 for NP. The results indicated that under the optimized conditions, the spiked recoveries were 86.20% - 106.20% （OP） and 81. 10% -91.80% （NP） , and the relative standard deviations（RSDs） for concentration of 0.1 mg/kg were 7.81% and 4.56% （n = 6）. The quantitation limits were 0.1 mg/kg. The method was simple, rapid and sensitive, and could meet the relevant requirement of international trades.

关 键 词：气相色谱一质谱 蚕丝制品 辛基酚 壬基酚 超声萃取 

分 类 号：TS101.9[轻工技术与工程—纺织工程]