加速溶剂萃取-液相色谱-质谱/质谱法分析动物组织中的壬基酚、辛基酚和双酚A

Analysis of Nonylphenol, Octylphenol and Bisphenol A in Animal Tissues by Liquid Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction

建立了测定内分泌干扰物质烷基酚、双酚A的液相色谱-电喷雾串联质谱(负离子模式)分析方法,优化了样品前处理方法.以二氯甲烷作提取溶剂,采用加速溶剂萃取法萃取动物组织样品,萃取液用500 mg OASIS氨基固相萃取柱进行浓缩净化.对流动相组分和流动相添加剂对质谱的离子化效率进行了考察,测得3种化合物在高、中、低3个添加水平的回收率为88% ～101% ,相对标准偏差小于15% ;双酚A、壬基酚和辛基酚的方法检出限分别为0.3, 0.05和0.1 μg/kg.对从北京市场上采集的27份动物组织样品进行检测,结果表明壬基酚广泛存在于各种动物源性食品中,检出含量为0.49～55.98 μg/kg,其中鱼肉组织中都检出壬基酚,而且其含量也较高(9.13～55.98 μg/kg).

A comprehensive analytical method based on liquid chromatography-electrospray ionization tandem mass spectrometry with negative ionization mode has been developed for measuring alkylphenols （AP） and bisphenol A （BPA） in animal tissues. Samples of animal tissues were extracted by accelerated solvent extraction with dichloromethane. Sample concentration and purification were performed using an OASIS NH2 solid extraction cartridge. The effects of mobile phase and additives on ionization were assessed. The recoveries for the compounds ranged from 88% to 101% and the relative standard deviations were below 15%.The detection limits of the method under multiple-reaction monitoring mode were 0.3,0.05 and 0. 1μg/kg for BPA, nonylphenol （NP） and octylphenol （OP）, respectively. The contents of NP ranging from 0.49 to 55.98 μg/kg were found in 27 real samples of animal tissues from Beijing market. The results indicate that the endocrine disrupting nonylphenol is ubiquitous in food of animal origin. Nonylphenol was found in all fish samples with concentration levels ranging from 9. 13 to 55.98 μg/kg.