顶空-气相色谱-质谱法测定涂饰皮革和合成革中二甲基甲酰胺的残留量研究
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摘要
采用顶空-气相-质谱法测定涂饰皮革及合成革中N,N-二甲基甲酰胺的残留量。样品经剪碎后,称取1 g在130℃顶空温度下加热50 min,采用VF-Wax色谱柱分离,外标法定量。本法检测低限可达0.1μg,平均回收率在89%以上,相对标准偏差在2.1%-4.6%。研究结果表明该方法灵敏度高、简便、准确,可用于DMF的检测。
Headspace-GC-MS was spplied for simuluaneous determination of residual DMF in garnish leather and synthetic leather. After being cut to pieces, 1 g of sample was heated at the headspace temperature of 130 for 50 min.then the headspace gas was separated with VF-Wax column. External standard method was used for quantification. The limits of detection of DMF was 0.1μg. The average recoveries were over89% and the relative standard deviation(RSD) were in the range of 2.1%-4.6%. This method is sensttive,simple,accurate and suitable for the determination of DMF.
Headspace-GC-MS was spplied for simuluaneous determination of residual DMF in garnish leather and synthetic leather. After being cut to pieces, 1 g of sample was heated at the headspace temperature of 130 for 50 min.then the headspace gas was separated with VF-Wax column. External standard method was used for quantification. The limits of detection of DMF was 0.1μg. The average recoveries were over89% and the relative standard deviation(RSD) were in the range of 2.1%-4.6%. This method is sensttive,simple,accurate and suitable for the determination of DMF.
引文
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[2]应杏秋,李峰,洪萍,等.尿中N,N-二乙基甲酰胺及其代谢物N-甲基乙酰胺的气相色谱测定法[J].中国卫生检验杂志,2011,21(11):2627-2628.
[3]苑金岐.二甲基乙酰胺市场调研报告[J].化工科技市场,2004,27(2):28-30.
[4]余文静,郑晨,张嵘,等.气相色谱/质谱联用检测化妆品中N,N-二乙基甲酰胺的残留[J].香料香精化妆品,2013,6:33-36.
[5]GLKENNEDY J R.Biological effects of acctamide,formamide,and their mono and dimethyl derivatives:an update[J].Crit.R ev.Toxicol.,2001,31(2):139-222.
[6]KIM S N.Preclinical toixicology and pharmacology of dimethylacetamide with clinical notes[J].Drug Metab.R ev.,1988,19(3):345-368.
[7]郑步云,王明龙,孙扣红.一例疑似职业性二甲基乙酰胺中毒的调查分析[J].职业卫生与应急救援,2010,28(5):259-260.
[8]徐艳琼,王建锋,龚伟.二甲基乙酰胺对职业暴露人群肝肾损害性别差异分析[J].职业与健康,2010,26(23):2750-2751.
[9]张亮,刘芳君.2例二甲基乙酰胺致急性肝病的分析报告[J].华南预防医学,2011,37(2):52-53.
[10]田丙正,张付海,张敏,等.高效液相色谱法测定合成革废气中N,N-二甲基甲酰胺.理化检验-化学分册[J],2017,,53(11):1300-1303.
[11]邓宜坤.高效液相色谱法测定合成革中N,N-二甲基甲酰胺[J].西部皮革,2018,5:28-29.