在线 MSPD-SPE-HPLC/FLD 分析牛组织中的多环芳烃。
On-line MSPD-SPE-HPLC/FLD analysis of polycyclic aromatic hydrocarbons in bovine tissues.
机构信息
Laboratorio de Análisis de Trazas, Departamento de Química Analítica, Facultad de Química de la Universidad Nacional Autónoma de México (UNAM), Ciudad Universitaria, 04510, Mexico; Departamento de Química, Facultad de Ciencias Naturales, Exactas y de la Educación, Universidad del Cauca, Sector Tulcán, 190003 Popayán, Colombia.
Laboratorio de Análisis de Trazas, Departamento de Química Analítica, Facultad de Química de la Universidad Nacional Autónoma de México (UNAM), Ciudad Universitaria, 04510, Mexico.
出版信息
Food Chem. 2017 May 15;223:82-88. doi: 10.1016/j.foodchem.2016.11.099. Epub 2016 Nov 22.
A fast method was optimized and validated for simultaneous trace determination of four polycyclic aromatic hydrocarbons: benzo[a]anthracene, benzo[b]fluoranthene, benzo[k]fluoranthene and benzo[a]pyrene in bovine tissues. The determination was performed by matrix solid-phase dispersion (MSPD) coupled on-line to solid phase extraction (SPE) and high performance liquid chromatography (HPLC) with fluorescence detection (FLD). The sample was dispersed on C silica sorbent and then the on-line MSPD-SPE-HPLC/FLD method was applied. Several parameters were optimized: cleaning and elution sequences applied to the MSPD cartridge, the flow rate and dilution of extract used for SPE loading. The on-line method was validated over a concentration range of 0.1-0.6ngg obtaining good linearity (r⩾0.998) and precision (RSD)⩽10%. Recovery ranged from 96 to 99% and the limits of detection were 0.012ngg. This methodology was applied to liver samples from unhealthy animals. The results demonstrate that MSDP-SPE-HPLC/FLD method provides reliable, sensitive, accurate and fast data to the food control.
一种快速方法被优化和验证，用于同时痕量测定牛组织中的四种多环芳烃：苯并[a]蒽、苯并[b]荧蒽、苯并[k]荧蒽和苯并[a]芘。测定采用基质固相分散（MSPD）与固相萃取（SPE）在线联用，高效液相色谱（HPLC）荧光检测（FLD）。样品在 C 硅胶吸附剂上分散，然后应用在线 MSPD-SPE-HPLC/FLD 方法。优化了几个参数：MSPD 小柱的清洗和洗脱顺序、SPE 加载用萃取物的流速和稀释度。在 0.1-0.6ngg 的浓度范围内进行了在线方法验证，得到了良好的线性（r ⩾ 0.998）和精密度（RSD） ⩽ 10%。回收率范围为 96-99%，检测限为 0.012ngg。该方法应用于来自不健康动物的肝脏样品。结果表明，MSDP-SPE-HPLC/FLD 方法为食品控制提供了可靠、灵敏、准确和快速的数据。
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