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建立了革材中N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAC)和N-甲基吡咯烷酮(NMP)3种有害溶剂残留量的气相色谱-质谱(GC-MS)同时测定方法。以甲醇为萃取剂,超声萃取后滤膜净化,再用GC-MS测试分析,外标法定量。在浓度0.1~20mg/L范围内3种目标物的线性关系良好,方法检出限在1.2~1.6mg/kg之间。以空白样品为基质,进行4个添加水平6次平行试验,结果表明:3种目标物的平均回收率均在85%~105%范围内,相对标准偏差(RSD)均小于6%。采用该方法测试了20个实际革材样品中DMF、DMAC和NMP残留量,其中皮革样品检出分别为75.2~539.2mg/kg、4.3~44.4mg/kg和5.0~25.7mg/kg;合成革样品检出分别为82.2~342.5mg/kg、8.6~78.8mg/kg和6.9~7.2mg/kg。
A gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of the residues of three hazardous solvents in leather, including N, N-dimethylformamide (DMF), N, N- dimethylacetamide (DMAC) and N-methylpyrrolidone (GC-MS) simultaneous determination method. Using methanol as extractant, the membrane was purified by ultrasonic extraction and then analyzed by GC-MS. The linearity of the three targets in the range of 0.1 ~ 20mg / L was good, and the detection limit was between 1.2 ~ 1.6mg / kg. The results showed that the average recoveries of all the three target species ranged from 85% to 105% with relative standard deviations (RSDs) less than 6%. The method was used to test the residual amount of DMF, DMAC and NMP in 20 real leather samples, including 75.2-593.2 mg / kg, 4.3-44.4 mg / kg and 5.0-25.7 mg / kg for leather samples respectively; Samples were detected 82.2 ~ 342.5mg / kg, 8.6 ~ 78.8mg / kg and 6.9 ~ 7.2mg / kg.