CAJ | 학술논문

建立了一个同时测定皮革及其制品中5种限用酰胺类溶剂残留量的气质联用方法。该方法以乙酸乙酯为萃取溶剂，超声萃取皮革及其制品中残留的限用酰胺类溶剂，萃取物经固相萃取柱净化后直接进行气相色谱/质谱-选择离子监测法测定，外标法定量。在信噪比(S/N)=3的条件下，甲酰胺、N-甲基甲酰胺、N,N-二甲基甲酰胺、N-甲基乙酰胺、N,N-二甲基乙酰胺的检出限分别为50、10、25、10、5 g/kg。在3个不同加标水平下，平均加标回收率为85.67%~95.23%，相对标准偏差为1.27%~4.36%(n=9)。该方法简便快速，灵敏度高，检出限远远低于REACH法规的限量要求，可完全满足皮革及其制品中限用酰胺类溶剂残留量检测工作的需要。
건립료일개동시측정피혁급기제품중5충한용선알류용제잔류량적기질련용방법。해방법이을산을지위췌취용제，초성췌취피혁급기제품중잔류적한용선알류용제，췌취물경고상췌취주정화후직접진행기상색보/질보-선택리자감측법측정，외표법정량。재신조비(S/N)=3적조건하，갑선알、N-갑기갑선알、N,N-이갑기갑선알、N-갑기을선알、N,N-이갑기을선알적검출한분별위50、10、25、10、5 g/kg。재3개불동가표수평하，평균가표회수솔위85.67%~95.23%，상대표준편차위1.27%~4.36%(n=9)。해방법간편쾌속，령민도고，검출한원원저우REACH법규적한량요구，가완전만족피혁급기제품중한용선알류용제잔류량검측공작적수요。
A gas chromatography/mass spectrometry method was established for the simultaneous determina-tion of the residual contents of 5 kinds of banned amides in leather and leather products. Residual banned amides in leather and leather products were ultrasonically extracted with ethyl acetate as the extraction sol-vent. The extract was purified by solid phase extraction column, and then was analyzed by gas chromatogra-phy/mass spectrometry-selected ion monitoring (GC/MS-SIM) technique. The concentration of each analyte was calibrated by the external standard method. The limit of detection (LOD) was 50, 10, 25, 10, 5 mg/kg for formamide, N-methylformamide, N,N-dimethyl formamide, N-methylacetamide and N,N-dimethylacetamide, respectively. Average spiked recoveries varied from 85.67% to 95.23% under three different spiked levels while the relative standard deviation (RSD) changed from 1.27%to 4.36%. The proposed method was simple, rapid and accurate, and the limits of detection (LOD) much less than the limited requirements of Regulation concerning registration, evaluation, authorization and restriction of chemicals (REACH). It could satisfy com-pletely the demand of determination of residual banned amides in leather and leather products.