首页|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)

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)

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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.
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.

Polycyclic Aromatic Hydrocarbons(PAHs)pollutantinternal standard methodhigh performance liquid chromatographyspices

侯美玲、冯桂蓉、蔡小钦、黄丹丹、董宪兵

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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

多环芳烃 污染物 内标法 高效液相色谱 香辛料

重庆市市场监督管理局科研计划项目

CQSJKJ2022006

2024

现代食品科技
华南理工大学

现代食品科技

CSTPCD北大核心
影响因子:1.07
ISSN:1673-9078
年,卷(期):2024.40(4)
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