高效液相色谱法测定皮革中20种溴代阻燃剂  

Determination of 20 kinds of brominated flame retardants in leather by HPLC method

作　　者：张瑞 张志辉[2] 刘卓钦[2] 梁金玲[2] 黎嘉明[2] 洗丽英 

机构地区：[1]从化出入境检验检疫局,广州510900 [2]广东出入境检验检疫局技术中心,广州510623

出　　处：《分析试验室》2014年第1期73-77,共5页Chinese Journal of Analysis Laboratory

基　　金：出入境检验检疫行业标准制(修)订计划项目(2012B102);广东检验检疫局科技计划项目(2013GDK17)资助

摘　　要：建立了皮革中20种多溴联苯和多溴联苯醚阻燃剂的高效液相色谱测定方法。采用y（二氯甲烷）：y（正己烷）=3：2混合溶剂作为提取溶剂，常温超声萃取30min，经硅胶固相萃取柱净化，蒸发浓缩至近干后用甲苯定容。用甲醇一缓冲溶液（pH7）为流动相梯度洗脱，C18反相萃取柱分离目标物质，于226nm检测。通过优化色谱梯度洗脱条件，有效排除了溶剂峰对低取代物的干扰。结果表明，目标物质质量浓度在5．0～25．0mg／L范围内线性关系良好，相关系数大于0．996，定量限（S／N=10）为5．20～41．7mg／kg，选定物质六溴联苯和十溴联苯醚的加标回收率为91．3％-102．9％。该法对所采用的20种目标物质中的16种都具有良好的分离效果，且对高溴代物的响应较好，可弥补气相色谱法对高溴代物灵敏度低的问题。方法可用于皮革中多溴联苯和多溴联苯醚的检测。A procedure was established for the determination of 20 kinds of polybrominated biphenyls （PBBs） and polybrominated diphenyl ether （PBDEs） flame retardants in leather by high performance liquid chromatogra- phy. With dichloromethane-hexane （ V/V = 3：2） mixed solvent as an extraction medium, samples were ultrasoni- cally extracted for 30 min at room temperature, followed by silica gel solid phase extraction （SPE） and evaporat- ed to nearly dry, and then marked to volume with toluene. The mobile phase was methanol-buffer solution （pHT） with ClS reversed phase column to analyze the target substances at 226 nm. By optimizing the chromato- graphic elution gradient, the interference of solvent peak with the low substituted substance peaks was effectively excluded. The results showed that the calibration curves presented good linear relationship at the concentration range of 5.0 ~ 25.0 mg/L, with the correlation coefficients greater than 0. 996. The limits of quantification （S/N = 10） were 5.20 -41.68 mg/kg, and recoveries for the selected materials of hexabromobiphenyl and de- cabromobiphenyl ether were 91.3% ~ 102.9%. The method have a good separation effect to 16 of 20 target sub-stances, and with good response for high bromide substituted substance, which means that it can compensate for the problem of gas chromatography of low sensitivity with high bromide substituted substance. The method can be used for determining PBBs and PBDEs in leather.

关 键 词：皮革 高效液相色谱 多溴联苯 多溴联苯醚 

分 类 号：O657.7[理学—分析化学]