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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: ; ; ; ; ; (邱思聪); (林家奎);

机构地区: 广东出入境检验检疫局

出  处: 《纺织学报》 2014年第5期91-96,共6页

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

领  域: [轻工技术与工程] [轻工技术与工程]

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