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

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。

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

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.