液相色谱-串联质谱法同时测定纺织品和食品包装材料中的壬基酚、辛基酚和双酚A

Simultaneous Determination of Nonylphenol,Octylphenol and Bisphenol A in Textiles and Food Packaging Materials by Liquid Chromatography Tandem Mass Spectrometry

建立了纺织品和食品包装材料中壬基酚、辛基酚和双酚A的液相色谱-串联质谱分析方法。不同类型的纺织品和食品包装材料样品采用加速溶剂萃取法,以无水乙醇为提取剂,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,收集甲醇-二氯甲烷(1∶4,V/V)洗脱液,采用Waters XBridge C18色谱柱,以甲醇-0.1%氨水溶液为流动相,梯度洗脱分离后,在LC/MS/MS多反应监测模式下进行定性与定量分析。壬基酚、辛基酚和双酚A的方法检出限为0.5μg/kg,在0.5～10μg/kg的3个添加水平范围内,纺织品样品的平均回收率为86.9%～92.5%,相对标准偏差均小于9.1%;食品包装材料样品的平均回收率为87.8%～93.0%,相对标准偏差均小于8.8%。本方法准确、快速、灵敏度高,可用于纺织品和食品包装材料的实际检验。

A comprehensive analytical method based on liquid chromatography tandem mass spectrometry has been developed for the determination of nonylphenol,octylphenol and bisphenol A in textiles and food packaging materials.Various textile and food packaging material samples were extracted under the conditions of 10.3 MPa and 120 ℃ by accelerated solvent extraction method with two static cycles using ethanol as the extraction solvent.The extract was cleaned up by Supelclean Envi-Carb solid phase extraction cartridge.Qualitative and quantitative analyses were carried out for the analytes under the multiple reaction monitoring（MRM） mode after the chromatographic separation on Waters XBridge C_18（150 mm×2.1 mm,3.5 μm） column with methanol-0.1% NH4OH gradient elution.The limits of detection（LODs） for alkylphenol,octyphenol and bisphenol A were 0.5 μg/kg.The mean recoveries for textile samples at the spiked level of 0.5-10 μg/kg were 86.9%-92.5%,with the relative standard deviation less than 9.1%.The mean recoveries for food packaging material samples at the spiked level of 0.5-10 μg/kg were 87.8%-93.0%,with the relative standard deviation less than 8.8%.The method is accurate,simple,rapid,and adapts to the inspection of nonylphenol,octylphenol and bisphenol A in textiles and food packaging materials.