气相色谱-质谱联用法测定OEKO-TEX皮革中的5种溶剂残留  

Determination of 5 Solvent Residues in OEKO-TEX Leather by Gas Chromatography Mass Spectrometry

作　　者：蔚彪 吴秀芳 白子竹 韩军 杨萌 董汉松 YU Biao;WU Xiufang;BAI Zizhu;HAN Jun;YANG Meng;DONG Hansong(National Textile and Leather Products Quality Supervision Testing Center,Beijing Product Quality Supervision and Inspection Institute,Beijing 100025,China)

机构地区：[1]北京市产品质量监督检验研究院国家纺织及皮革产品质量监督检验中心,北京100025

出　　处：《中国皮革》2023年第11期1-6,共6页China Leather

摘　　要：建立了气相色谱-质谱联用技术同时测定OEKO-TEX皮革标准中列举的甲酰胺、N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMA)、N-甲基吡咯烷酮(NMP)和N-乙基吡咯烷酮(NEP)5种高度关注物质的方法,并就样品前处理条件和色谱条件进行了优化:以乙腈为提取溶剂,50℃超声提取60 min。方法线性范围0.13~6.76μg/mL,相关系数0.9992~0.9999,方法检出限0.03~0.26 mg/kg,加标回收率79.78%~111.51%,相对标准偏差1.52%~5.74%。市售的皮革测定结果显示,检出率为51.16%,其中DMF检出率最高,DMA次之,甲酰胺、NMP和NEP检出率最低。A method for the simultaneous determination of formamide, N,N-dimethylformamide(DMF), N,N-dimethylacetamide(DMA), N-methyl-pyrrolidone(NMP) and N-ethyl-pyrrolidone(NEP) listed in the OEKO-TEX leather standard by gas chromatography-mass spectrometry was established. The sample pretreatment conditions and chromatographic conditions were optimized: acetonitrile was used as the extraction solvent, and ultrasonic extraction at 50 ℃ for 60 minutes. The linear range of the method is 0.13~6.76 μg/mL, correlation coefficient 0.999 2~0.999 9, detection limit 0.03~0.26 mg/kg, spiked recovery 79.78%~111.51%, relative standard deviation 1.52%~5.74%. The detection rate of leather sold in the market was 51.16%. DMF was the highest, followed by DMA, and formamide, NMP and NEP were the lowest.

关 键 词：溶剂残留 气质联用仪 酰胺 吡咯烷酮 

分 类 号：TS57[轻工技术与工程—皮革化学与工程]