皮革与化工
皮革與化工
피혁여화공
LEATHER AND CHEMICALS
2015年
2期
1-5,22
,共6页
王成云%唐莉纯%邬晓慧%李燕华%林镱琳%沈雅蕾%林君峰%谢堂堂
王成雲%唐莉純%鄔曉慧%李燕華%林鐿琳%瀋雅蕾%林君峰%謝堂堂
왕성운%당리순%오효혜%리연화%림의림%침아뢰%림군봉%사당당
微波辅助萃取%酰胺%皮革%气相色谱/质谱-选择离子监测法
微波輔助萃取%酰胺%皮革%氣相色譜/質譜-選擇離子鑑測法
미파보조췌취%선알%피혁%기상색보/질보-선택리자감측법
microwave-assisted extraction%amide%leather%gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM)
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。
以甲醇為萃取溶劑,採用微波輔助萃取技術提取皮革及其製品中殘留的限用酰胺類溶劑,提取液經固相萃取柱淨化後進行氣相色譜/質譜-選擇離子鑑測法測定,外標法定量,從而建立瞭1箇同時測定皮革及其製品中5種限用酰胺類溶劑的氣質聯用方法。在信譟比(S/N)=3的條件下,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-二甲基乙酰胺的檢齣限分彆為50、10、10、25、5μg/kg。在3箇不同加標水平下,平均加標迴收率為86.13%~95.67%,相對標準偏差1.35%~4.28%(n=9)。該方法簡單快捷,靈敏度高,檢齣限低,適用于皮革及其製品中限用酰胺類溶劑殘留量的檢測。
이갑순위췌취용제,채용미파보조췌취기술제취피혁급기제품중잔류적한용선알류용제,제취액경고상췌취주정화후진행기상색보/질보-선택리자감측법측정,외표법정량,종이건립료1개동시측정피혁급기제품중5충한용선알류용제적기질련용방법。재신조비(S/N)=3적조건하,갑선알、N-갑기갑선알、N-갑기을선알、N,N-이갑기갑선알、N,N-이갑기을선알적검출한분별위50、10、10、25、5μg/kg。재3개불동가표수평하,평균가표회수솔위86.13%~95.67%,상대표준편차1.35%~4.28%(n=9)。해방법간단쾌첩,령민도고,검출한저,괄용우피혁급기제품중한용선알류용제잔류량적검측。
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.