短链氯化石蜡( SCCPs)是我国皮革加脂过程中常用的添加剂,但近年已被欧盟等列为禁止使用的持久性有机污染物。由于 SCCPs结构复杂,且皮革基质干扰严重,目前尚没有完善的皮革制品中 SCCPs 的标准检测方法。本文采用硅胶为固相萃取柱萃取,以正己烷-二氯甲烷(2∶1,v/v)为洗脱剂,使 SCCPs与皮革基质中的干扰组分完全分离,建立了用于测定皮革制品中 SCCPs 的固相萃取-气相色谱-质谱方法。该方法的回收率为90.47%~99.00%,检出限为0.069~0.110 mg/kg,相对标准偏差( RSD)为4.20%~6.69%。该方法适用于皮革中 SCCPs 的定性、定量分析。
The short chain chlorinated paraffins( SCCPs)are the additives frequently used in the leather production in China,but they have been put into the list of forbidden chemicals issued by European Union recently. In fact,there is not a commonly recognized method for the determination of the SCCPs in the leather products due to the serious matrix interferences from the leather products and the complex chemical structures of the SCCPs. A method of solid phase extraction coupled with gas chromatography-mass spectrometry ( SPE-GC-MS ) was established for the determination of the SCCPs in the leather products after the optimization of the SPE conditions. It was found that the interferences from the leather products were thor-oughly separated from the analyte of the SCCPs on a home-made solid phase extraction( SPE) column filled with silica packing while eluted with a mixed solvent of n-hexane-methylene chlo-ride(2∶1,v/v). With this method,the recoveries for the SCCPs spiked in the real leather sam-ples varied from 90. 47% to 99. 00% with the relative standard deviations( RSDs)less than 6. 7%,and the limits of detection( LODs)were between 0. 069 and 0. 110 mg/kg. This method is suitable for qualitative and quantitative analysis of SCCPs in the leather products.
参考文献
[1] | Santos F J;Parera J;Galceran M T.[J].Analytical Biochemistry,2006386(04):837. |
[2] | 张海军;高媛;马新东.[J].中国科学:化学,201343(03):255. |
[3] | Zencak Z;Oehme M.[J].Trends in Analytical Chemistry,200625(04):310. |
[4] | Llorca-PorcellJ;Martínez-Soriano E;Valor I.[J].Journal of Separation Science,200932:1425. |
[5] | Pellizzato F;Ricci M;Held A.[J].Journal of Environmental Monitoring,20079:924. |
[6] | Castells P;Santos F J;Galceran M T.[J].Journal of Chromatography A,20041025(02):157. |
[7] | Castells P;Santos F J;Galceran M T.[J].Journal of Chromatography A,2003984(01):1. |
[8] | Iozza S;Müller C E;Schmid P.[J].Environmental Science and Technology,200842(04):1045. |
[9] | Gao Y;Zhang H;Chen J.[J].Analytica Chimica Acta,2011703(02):187. |
[10] | SN/T2570-2010.[S]. |
[11] | 花金龙;廖帼英;杨欣卉.[J].皮革科学与工程,201222(04):66. |
[12] | 马贺伟.[J].中国皮革,201241(21):1. |
[13] | 马贺伟.[J].皮革科学与工程,201222(06):67. |
[14] | Rey A;Blanc N;Cannot J C.[J].Journal of the American Leather Chemists Association,2011106(10):294. |
- 下载量()
- 访问量()
- 您的评分:
-
10%
-
20%
-
30%
-
40%
-
50%