旋涡辅助-柱前衍生-气相色谱-串联质谱法测定木砧板及木筷子中的五氯酚  

Determination of pentachlorophenol in wooden chopping boards and wooden chopsticks by vortex-assisted pre-column derivatization gas chromatography-tandem mass spectrometry

作　　者：兰红军[1] 吴雪梅[1] 冯耀基[1] 黎少映 LAN Hongjun;WU Xuemei;FENG Yaoji;LI Shaoying(Nanhai Center for Disease Prevention and Control,Guangdong Foshan 528200,China)

机构地区：[1]佛山市南海区疾病预防控制中心

出　　处：《中国食品卫生杂志》2019年第3期231-236,共6页Chinese Journal of Food Hygiene

基　　金：佛山市南海区“十三五”重点专科(特色专科)建设项目

摘　　要：目的建立旋涡辅助-柱前衍生-气相色谱-串联质谱(GC-MS/MS)法测定木砧板及木筷子中五氯酚的方法。方法加入硫酸溶液,使五氯酚钠转化为分子态的五氯酚,以乙酸乙酯-正己烷混合溶剂(2∶8,V/V)萃取,浓硫酸净化,加入乙酸酐吡啶溶液衍生。采用HP-5MS色谱柱(30 m×0.25 mm,0.25μm)进行分离,GC-MS-MS多反应监测(MRM)测定。结果在0~200μg/L范围内,五氯酚具有良好的线性关系(r=0.999 8),检出限为0.2μg/kg,定量限为0.7μg/kg。在高、中、低3个浓度水平下,平均加标回收率为90.0%~103.6%,相对标准偏差(RSD)为1.5%~3.6%(n=6)。结论本方法具有准确性高、灵敏度高、快速等特点,适用于木砧板及木筷子中五氯酚的准确检测。Objective To establish a method for the determination of pentachlorophenol in wooden chopping boards and wooden chopsticks by vortex-assisted pre-column derivatization gas chromatography-tandem mass spectrometry(GC-MS/MS). Methods The sulfuric acid solution was added to convert sodium salt into molecular pentachlorophenol, which was extracted with a mixed solvent of ethyl acetate and n-hexane(2∶8,V/V), purified by concentrated sulfuric acid, and derivatized with acetic acid pyridine solution. HP-5 MS column(30 m×0.25 mm,0.25 μm) was used for separation and GC-MS/MS multiple reaction monitoring(MRM) was used for determination. Results In the range of 0-200 μg/L, pentachlorophenol had a good linear relationship(r=0.999 8), the detection limit was 0.2 μg/kg, and the limit of quantification was 0.7 μg/kg. The recoveries and precisions of the three concentrations(n=6) showed an average spike recovery ranged from 90.0% to 103.6% with the relative standard deviation(RSD) of 1.5%-3.6%. Conclusion This method was accurate, highly sensitive and rapid. It is suitable for the accurate detection of pentachlorophenol in wooden chopping boards and wooden chopsticks.

关 键 词：五氯酚 柱前衍生 气相色谱-串联质谱法 木砧板 木筷子 

分 类 号：R155[医药卫生—营养与食品卫生学]