色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
10期
1152-1156
,共5页
张伟亚%万昕%李丽霞%王成云%金淑培%邢钧
張偉亞%萬昕%李麗霞%王成雲%金淑培%邢鈞
장위아%만흔%리려하%왕성운%금숙배%형균
固相萃取%气相色谱-质谱法(GC-MS)%短链氯化石蜡( SCCPs)%皮革制品
固相萃取%氣相色譜-質譜法(GC-MS)%短鏈氯化石蠟( SCCPs)%皮革製品
고상췌취%기상색보-질보법(GC-MS)%단련록화석사( SCCPs)%피혁제품
solid phase extraction( SPE)%gas chromatography-mass spectrometry( GC-MS)%short chain chlorinated paraffins( SCCPs)%leather products
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。
短鏈氯化石蠟( SCCPs)是我國皮革加脂過程中常用的添加劑,但近年已被歐盟等列為禁止使用的持久性有機汙染物。由于 SCCPs結構複雜,且皮革基質榦擾嚴重,目前尚沒有完善的皮革製品中 SCCPs 的標準檢測方法。本文採用硅膠為固相萃取柱萃取,以正己烷-二氯甲烷(2∶1,v/v)為洗脫劑,使 SCCPs與皮革基質中的榦擾組分完全分離,建立瞭用于測定皮革製品中 SCCPs 的固相萃取-氣相色譜-質譜方法。該方法的迴收率為90.47%~99.00%,檢齣限為0.069~0.110 mg/kg,相對標準偏差( RSD)為4.20%~6.69%。該方法適用于皮革中 SCCPs 的定性、定量分析。
단련록화석사( SCCPs)시아국피혁가지과정중상용적첨가제,단근년이피구맹등렬위금지사용적지구성유궤오염물。유우 SCCPs결구복잡,차피혁기질간우엄중,목전상몰유완선적피혁제품중 SCCPs 적표준검측방법。본문채용규효위고상췌취주췌취,이정기완-이록갑완(2∶1,v/v)위세탈제,사 SCCPs여피혁기질중적간우조분완전분리,건립료용우측정피혁제품중 SCCPs 적고상췌취-기상색보-질보방법。해방법적회수솔위90.47%~99.00%,검출한위0.069~0.110 mg/kg,상대표준편차( RSD)위4.20%~6.69%。해방법괄용우피혁중 SCCPs 적정성、정량분석。
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.