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

纺织学报 ›› 2014, Vol. 35 ›› Issue (5): 91-0.

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

李淳¹ 邱思聪² 任忠海¹ 梁文杰² 余林³ 曹维强^2，3 林家奎⁴

1. 广东出入境检验检疫局
2. 惠州出入境检验检疫局
3. 广东工业大学轻工化工学院
4. 广东省丝绸纺织集团有限公司

收稿日期:2013-06-06 修回日期:2013-11-08 出版日期:2014-05-15 发布日期:2014-05-09
通讯作者: 曹维强 E-mail:caowqciq@163.com
基金资助:
广东省科技计划项目

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

Received:2013-06-06 Revised:2013-11-08 Online:2014-05-15 Published:2014-05-09

摘要/Abstract

摘要： 建立了固相萃取气相色谱-质谱法同时测定蚕丝制品中辛基酚(OP)、壬基酚(NP)的分析方法，并对提取溶剂的选择、提取方式、固相萃取条件以及气相色谱质谱条件进行了研究。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,采用气相色谱质谱进行检测, 定量离子分别为m /z107，定性离子分别为m /z206（OP）和m /z220 ( NP)。在优化实验条件下, 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%（OP）和81.10%-91.80%（NP）, 相对标准偏差分别为7.81%和4.56% (0.1mg/kg, n=6)。方法简单、快速、灵敏度高, 可满足国际贸易过程中对蚕丝制品中OP、NP的测定要求。

关键词: 气相色谱-质谱, 蚕丝制品, 辛基酚, 超声萃取

Abstract: Abstract: A method was developed for measurement of octylphenol(OP) and nonlyphenol (NP) residues in textile products by gas chromatography-mass spectrometry， which studied the choice of extraction solvent, extracting methods, solid phase extraction conditions and conditions of gas chromatography-mass spectrometry. The study showed that the OP and NP in textile products 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/z107 for OP and NP, and qualitative ions were selected at m/z206 for OP and m/z220 for NP. The results indicated that under the optimized conditions, the spiked recoveries were 86.20%-106.20%（OP）and 81.10%-91.80%（OP）, and the relative standard deviations(RSDs) for concentration of 0.1mg /kg were 7.81% and 4.56% ( n = 6) . The quantitation limits were 0.1mg /kg. The method was simple, rapid and sensitive, and could meet the relevant requirement of European Union.

Key words: gas chromatography-mass spectrometry, silk product, octylphenol, nonlyphenol, ultrasonic-assisted extraction

李淳邱思聪任忠海梁文杰余林曹维强林家奎. 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[J]. 纺织学报, 2014, 35(5): 91-0.

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