首页> 中文期刊> 《皮革与化工》 >微波辅助萃取-气质联用法同时测定皮革及其制品中5种限用酰胺类溶剂的残留量

微波辅助萃取-气质联用法同时测定皮革及其制品中5种限用酰胺类溶剂的残留量

         

摘要

An effective method was established to determine the residual contents of five banned amides in leather and leather products simultaneously. Residual amides in leather and leather products were microwave-assisted extracted, using methanol as the extraction solvent. The extract was then purified by solid-phase extraction column, followed by the analysis of gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) technique. The concentration of each analyte were calibrated by external standard method. The limit of detection (LOD) was 50, 10, 10, 25 and 5 g/kg for formamide, N-methylformamide, N-methylacetamide, N,N-dimethylformamide and dimethylace-tamide, respectively, under the condition of signal to noise (S/N) of 3. The spiked average recoveries changed from 86.13% to 95.67% under three different spiked levels while the relative standard deviation (RSD) varied from 1.35%to 4.28%. The proposed method was simple, rapid, accurate and sensitive, and applicable for the determination of residual amides in leather and leather products.%以甲醇为萃取溶剂,采用微波辅助萃取技术提取皮革及其制品中残留的限用酰胺类溶剂,提取液经固相萃取柱净化后进行气相色谱/质谱-选择离子监测法测定,外标法定量,从而建立了1个同时测定皮革及其制品中5种限用酰胺类溶剂的气质联用方法。在信噪比(S/N)=3的条件下,甲酰胺、N-甲基甲酰胺、N-甲基乙酰胺、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺的检出限分别为50、10、10、25、5μg/kg。在3个不同加标水平下,平均加标回收率为86.13%~95.67%,相对标准偏差1.35%~4.28%(n=9)。该方法简单快捷,灵敏度高,检出限低,适用于皮革及其制品中限用酰胺类溶剂残留量的检测。

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