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高效液相色谱-荧光检测法测定水产品中15种多环芳烃
引用本文:孙秀梅,梅光明,陈雪昌,郭远明,陈朋.高效液相色谱-荧光检测法测定水产品中15种多环芳烃[J].南方水产,2012,8(3):48-53.
作者姓名:孙秀梅  梅光明  陈雪昌  郭远明  陈朋
作者单位:1. 浙江省海洋水产研究所,农业部渔业环境及水产品质最监督检验测试中心(舟山),浙江舟山316100
2. 新诺佳生物工程公司,浙江舟山,316101
基金项目:国家海洋公益性行业科研专项,浙江省海洋环保项目
摘    要:建立了高效液相色谱荧光检测法同时测定水产品中15种多环芳烃(polycyclic aromatic hydrocarbons,PAHs)的方法。通过液相色谱柱、荧光激发和发射波长等条件的优化,实现了15种多环芳烃组分基线完全分离和荧光高灵敏度检测。在优化的试验条件下,检测的15种多环芳烃中萘、苊和芴的检出限为0.5μg·kg^-1,苯并b]荧蒽、二苯并a.h]蒽和苯并g,h,i]茈的检出限为2.0μg·kg^-1,其余化合物的检出限为1.0μg·kg^-1;在检测的15种多环芳烃中,菲、蒽、芘、苯并a]蒽、崫、苯并a]芘、茚并1,2,3-cd]芘在0.001~0.500mg·L^-1质量浓度范围,其余化合物在0.002~1.000mg·L^-1质量浓度范围,呈良好的线性相关,相关系数R^2〉0.995;样品加标水平分别为2.0μg·kg、10.0μg·kg^-1和100.0μg·kg^-1时回收率为71.1%-98.4%,相对标准偏差(RSD)〈10%。该检测方法重现性高,检测灵敏度和准确度均满足分析要求。

关 键 词:多环芳烃  水产品  高效液相色谱  荧光法

Determination of 15 polycyclic aromatic hydrocarbons in aquatic products by HPLC-Fluorescence
SUN Xiumei , MEI Guangming , CHEN Xuechang , GUO Yuanming , CHEN Peng.Determination of 15 polycyclic aromatic hydrocarbons in aquatic products by HPLC-Fluorescence[J].South China Fisheries Science,2012,8(3):48-53.
Authors:SUN Xiumei  MEI Guangming  CHEN Xuechang  GUO Yuanming  CHEN Peng
Institution:1. Fishery Environment and Aquatic Products Quality Supervision Testing Center( Zhoushan), Ministry of Agriculture; Marine Fishery Institute of Zhefiang Province, Zhoushan 316100, China; 2. Sinomega Biotech Engineering Company, Zhonshan 316101, China)
Abstract:We used high performance liquid chromatography (HPLC) coupled to a fluorescence detector (FLD) to determine 15 polycyclie aromatic hydrocarbons (PAHs) in aquatic products and realized complete base-line separation of the 15 PAHs and high sensitive fluorescence determination based on optimization of liquid chromatographic conditions, excitation and emission wavelength. Under optimizing conditions, the detection limit of naphthalene, acenaphthene and fluorene is 0. 5 μg ·kg^-1 that of benzo (b) fluoranthene, dibenzo (a, h) anthracene and benzo (g, h, i) perylene is 2. 0 μg ·kg^-1 ; that of the others is 1. 0 μg ·kg^-1. PHE, AN, PY, BaA, CHR, BaP and IP are in the range of 0. 001 -0. 500 mg.L ^-1 , and the others are in the range of 0. 002 - 1. 000 mg·L ^-1 , having good linearity (R2 〉0.995). The recovery at the spiked amount of 2.0 μg ·kg^-1, 10.0 μg ·kg^-1and 100.0 μg ·kg^-1 is 71.1% -98.4% (RSD 〈10%). The reproducible, sensitive and accurate method is suitable for quality control of the 15 PAHs in aquatic products.
Keywords:polycyelic aromatic hydrocarbons  aquatic products  high perfornmnce liquid chromatography  fluorescence detection
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