方 丽,江 晓,李雪莹,张 丽,黄嘉颖,张方圆.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[J].食品安全质量检测学报,2024,15(2):74-82
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
投稿时间:2023-11-29  修订日期:2024-01-19
DOI:
中文关键词:  乌梅  多环芳烃  气相色谱-三重四极杆质谱联用法  蒸晒  熏制
英文关键词:mume fructus  polycyclic aromatic hydrocarbons  gas chromatography-triple quadrupole mass spectrometry  steam-dried  smoke-dried
基金项目:食品化学污染物样品绿色制备技术、广东省重点领域研发计划项目(2019B020211001)。
作者单位
方 丽 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 
江 晓 广东省食品药品职业技术学校 
李雪莹 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 
张 丽 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 
黄嘉颖 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 
张方圆 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 
AuthorInstitution
FAND Li 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) 
JIANG Xiao Guangdong Food and Drug Vocational College 
LI Xue-Ying 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) 
ZHANG Li 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) 
HUANG Jia-Ying 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) 
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) 
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中文摘要:
      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r2>0.997), 检出限(limits of detection, LODs)为0.05~0.40 μg/kg, 定量限(limits of quantitation, LOQs)为0.20~1.40 μg/kg, 在1、5和20 μg/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。
英文摘要:
      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 r2>0.997), and the limits of detection (LODs) were 0.05?0.40 μg/kg, the limits of quantitation (LOQs) were 0.20?1.40 μg/kg, the recoveries ranged from 63.3% to 119.0% at 3 different level of spiked samples of 1, 5 and 20 μg/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.
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