高效液相色谱-内标法测定香辛料中15种多环芳烃类污染物(PAHs)
Determination of 15 Polycyclic Aromatic Hydrocarbon(PAH)Pollutants in Spices by an Internal Standard High Performance Liquid Chromatography(HPLC)
侯美玲 1冯桂蓉 1蔡小钦 1黄丹丹 1董宪兵1
作者信息
- 1. 重庆市食品药品检验检测研究院,国家市场监管重点实验室(调味品监管技术),重庆 401121
- 折叠
摘要
该研究建立了高效液相色谱(High Performance Liquid Chromatography,HPLC)同时分析香辛料中15种多环芳烃类污染物(Polycyclic Aromatic Hydrocarbons,PAHs)含量的内标检测方法.样品经氢氧化钠溶解,乙腈萃取,正己烷复溶后,过弗罗里硅土(Florisil)小柱净化浓缩,供HPLC 检测,苯并[a]芘-D12 作为内标定量.该方法在0～100 ng/mL内线性关系良好,辣椒中PAHs检出限:0.5～3.0 μg/kg;定量限2.0～10.0 μg/kg;花椒中检出限:0.5～1.0 μg/kg;定量限2.0～3.0 μg/kg.在2.0、10.0、50.0 μg/kg 3个浓度水平,辣椒中回收率范围为60.58%～119.48%,相对标准偏差(Relative Standard Deviations,RSD)(n=6)为1.25%～9.61%,花椒中回收率为60.46%～119.24%,RSD(n=6)为1.10%～8.56%.5种地产香辛料中∑PAHs含量由高到低为:青花椒(561.2 μg/kg)＞二荆条(448.8 μg/kg)＞红花椒(358.3 μg/kg)＞石柱红(353.6 μg/kg)＞小米辣(243.5 μg/kg),区县种植基地污染较严重的为璧山、江津和荣昌,∑PAHs分别为721.5、626.6和621.0 μg/kg,PAHs中污染较严重的化合物为菲、荧蒽和芘,平均含量分别为215.10、80.25和75.35 μg/kg.该研究建立的内标法准确度高,重复性好,适用于香辛料及制品中PAHs检测.
Abstract
An internal standard HPLC method was established for simultaneous determination of 15 kinds of PAHs in spices by.The samples were dissolved in sodium hydroxide,extracted with acetonitrile,redissolved by n-hexane,cleaned and concentrated by the Florisil SPE cartridge,and determined by HPLC,with benzo[a]pyrene D12 being used as the internal standard.This method had a good linear relationship in the range of 0～100 ng/mL,with the detection limits of PAHs in Capsicum being 0.5～3.0 μg/kg and the limits of quantitation as 2.0～10.0 μg/kg.The limits of detection and limits of quantitation of PAHs in Zanthoxylum were 0.5～1.0 μg/kg and 2.0～3.0 μg/kg,respectively.When the spiked levels were 2.0,10.0 and 50.0 μg/kg,the recoveries in the two spices were 60.58%～119.48%and 60.46%～119.24%,with the RSD(n=6)being 1.25%～9.61%and 1.10%～8.56%.The concentration of ∑PAHs in the five spices from high to low were:green Zanthoxylum(561.2 ųg/kg)>erjingtiao(448.8 μg/kg)>red Zanthoxylum(358.3 μg/kg)>shizhuhongi(353.6 μg/kg)>chilli(243.5 μg/kg).The more seriously polluted areas of Chongqing were Bishan,Jiangjin and Rongchang,with ∑PAHs being 721.5,626.6 and 621.0 μg/kg,respectively.The more seriously polluted compounds in PAHs were phenanthrene,fluoranthrene and pyrene,with their average contents being 215.10,80.25 and 75.35 μg/kg,respectively.The internal standard method established in this study has high accuracy and good repeatability,which is suitable for the determination of PAHs in spices.
关键词
多环芳烃/污染物/内标法/高效液相色谱/香辛料Key words
Polycyclic Aromatic Hydrocarbons(PAHs)/pollutant/internal standard method/high performance liquid chromatography/spices引用本文复制引用
基金项目
重庆市市场监督管理局科研计划项目(CQSJKJ2022006)
出版年
2024
国家科技期刊平台
NSTL
万方数据