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

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

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.