气相色谱-三重四极杆质谱法同时测定乌梅中25种多环芳烃及其污染来源分析  

Simultaneous determination of 25 kinds of polycyclic aromatic hydrocarbons in mume fructus by gas chromatography-triple quadrupole mass spectrometry and their pollution source analysis

作　　者：方丽 江晓 李雪莹 张丽 黄嘉颖 张方圆 FAND Li;JIANG Xiao;LI Xue-Ying;ZHANG Li;HUANG Jia-Ying;ZHANG Fang-Yuan(Guangdong Provincial Engineering Research Center for Efficacy Component Testing and Risk Substance Rapid Screening of Health Food,Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology,Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,Guangzhou),Guangzhou 510070,China;Guangdong Food and Drug Vocational College,Guangzhou 510663,China)

机构地区：[1]广东省科学院测试分析研究所(中国广州分析测试中心),广东省化学测量与应急检测技术重点实验室,广东省保健食品功效成分检测与风险物质快速筛查工程技术研究中心,广州510070 [2]广东省食品药品职业技术学校,广州510663

出　　处：《食品安全质量检测学报》2024年第2期74-82,共9页Journal of Food Safety and Quality

基　　金：广东省重点领域研发计划项目(2019B020211001)。

摘　　要：目的建立气相色谱-三重四极杆质谱法(gas chromatography-triple quadrupole mass spectrometry,GC-MS/MS)同时测定乌梅中25种多环芳烃(polycyclic aromatic hydrocarbons,PAHs),并对污染来源进行分析。方法样品经二氯甲烷超声萃取,基质固相分散(matrix solid-phase dispersion,MSPD)净化,DB-EUPAH色谱柱分离,多反应监测(multiple reaction monitorin,MRM)采集,内标法定量。结果25种PAHs在1~500 ng/mL范围内线性良好(相关系数r 2>0.997),检出限(limits of detection,LODs)为0.05~0.40μg/kg,定量限(limits of quantitation,LOQs)为0.20~1.40μg/kg,在1、5和20μg/kg 3个浓度水平的加标回收率为63.3%~119.0%,相对标准偏差(relative standard deviations,RSDs)为2.2%~6.5%(n=6)。乌梅样品中除二苯并[a,h]芘(DBahP)外,其余24种PAHs均有检出,菲(Phe)、荧蒽(Flt)、芘(Pyr)的含量较高,蒸晒与熏制乌梅中PAHs的污染分布存在明显差异。结论本方法前处理操作简单、灵敏度高、方法稳定、抗干扰性强,可同时实现乌梅中25种PAHs的测定。Objective To establish a gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)method for simultaneous determination of 25 kinds of polycyclic aromatic hydrocarbons(PAHs)in mume fructus,and analyze their pollution source.Methods The samples were extracted by dichloromethane ultrasound,purified by matrix solid-phase dispersion(MSPD),separated by DB-EUPAH,collected by multiple reaction monitorin(MRM),and quantified by internal standard method.Results The linearity of 25 kinds of PAHs were good in the range of 1‒500 ng/mL(correlation coefficient r 2>0.997),and the limits of detection(LODs)were 0.05‒0.40μg/kg,the limits of quantitation(LOQs)were 0.20‒1.40μg/kg,the recoveries ranged from 63.3%to 119.0%at 3 different level of spiked samples of 1,5 and 20μg/kg with the relative standard deviations(RSDs)(n=6)range from 2.2%to 6.5%.The 25 kinds of PAHs were detected in the mume fructus samples,except for dibenzo[a,h]pyrene(DBahP),the content of phenanthrene(Phe),fluoranthene(Flu)and pyrene(Pyr)were high.There were obvious differences in the content and distribution of PAHs between the steamed and smoked products.Conclusion The method has simple pre-processing operation,high sensitivity,stable method,strong anti-interference ability,which can be used to determine 25 kinds of PAHs in mume fructus simultaneously.

关 键 词：乌梅 多环芳烃 气相色谱-三重四极杆质谱法 蒸晒 熏制 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]