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

Simultaneous Determination of the Residual Contents of Five Banned Amides in Leather and Leather Products by Gas Chromatography/Mass Spectrometry Combined with Microwave-assisted Extraction

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。

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.