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作 者:马强[1] 白桦[1] 王超[1] 张庆[1] 肖海清[1] 周新[1] 闫妍[1] 董益阳[1] 王宝麟[1]
出 处:《分析测试学报》2009年第10期1160-1164,共5页Journal of Instrumental Analysis
基 金:国家质量监督检验检疫总局科研项目资助(2007IK094)
摘 要:建立了高效液相色谱-二极管阵列检测器(DAD)/荧光检测器(FLD)串联技术同时测定纺织品和食品包装材料中壬基酚、辛基酚和双酚A的方法。实验样品采用加速溶剂萃取法,以无水乙醇为提取溶剂,在10.3 MPa和120℃下静态循环提取2次,提取液经Supelclean Envi-Carb石墨化碳黑固相萃取柱净化,以Agi-lent Zorbax SB-Phenyl(250 mm×4.6 mm,5μm)色谱柱分离后用DAD-FLD串联法进行检测。壬基酚、辛基酚和双酚A的DAD检测波长为225 nm;荧光激发波长为227 nm,发射波长为315 nm。在25、50、500μg/kg的添加水平下,纺织品样品和食品包装材料样品的平均回收率均为93%-98%,相对标准偏差分别为2.8%-7.0%和2.9%-6.9%。方法准确、简便、快速,可用于纺织品和食品包装材料的实际检验工作。An analytical method based on high performance liquid chromatography (HPLC) with diode array detector (DAD) and fluorescence detector (FLD) was developed for the determination of nonylphenols, octylphenols and bisphenol A in textiles and food packaging materials. Accelerated solvent extraction method was used to extract the analytes from various food packaging materials and textile samples under 10.3 MPa and 120 ℃with two static cycles using ethanol as the extraction solvent. The extract was cleaned up by Supelclean Envi-Carb solid phase extraction cartridge. After chromatographic separation on Agilent Zorbax SB-Phenyl (250 mm× 4.6 mm, 5 μm) column, the HPLC - DAD chromatogram of analytes was recorded at 225 nm and HPLC - FLD chromatogram at 315 nm( λex =227 nm). The mean recoveries for textile samples and food packaging material samples at three spiked levels were both 93% -98% , with RSDs of 2. 8% - 7.0% and 2.9% - 6.9% , respectively. The method is accurate, simple, rapid and feasible for the inspection of nonylphenol, octylphenol and bisphenol A in textiles and food packaging materials.
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