高效液相色谱-荧光检测法测定橄榄油中4种多环芳烃

建立了高效液相色谱-荧光检测(HPLC-FLD)测定橄榄油中苯并a]蒽、屈艹、苯并b]荧蒽、苯并a]芘4种多环芳烃(PAHs)的分析方法。橄榄油样品经异丙醇稀释,采用具有π-π特异性作用的固相萃取柱净化,Agilent ZORBAX Eclipse PAH色谱柱(100 m m×2.1 m m,1.8μm)分离,以水-乙腈为流动相,梯度洗脱,实现了4种化合物的基线分离,并用基质匹配校准溶液进行外标法定量。4种多环芳烃的线性范围为2.4~40μg/L,相关系数(r)为0.999 0~0.999 9,方法的定量限为0.147~0.413μg/L,加标回收率为95.5%~103.2%,日内和日间精密度(RSD)分别为0.10%~1.69%和2.48%~2.93%(n=5)。该法具有灵敏度高、检出限低、重复性好等特点,适用于橄榄油中4种PAHs快速、准确的定量检测。

Determination of four polycyclic aromatic hydrocarbons in olive oil by high performance liquid chromatography-fluorescent detection

A method for the determination of four polycyclic aromatic hydrocarbons (PAHs) such as benzoa]anthracene, chrysene, benzob]fluoranthene and benzoa]pyrene in olive oil by high performance liquid chromatography-fluorescent detection (HPLC-FLD) was developed. The olive oil samples were diluted with isopropanol and cleaned-up by a solid phase extraction cartridge with π-π specificity. Critical isomers were separated by gradient elution with water-acetonitrile on an Agilent ZORBAX Eclipse PAH column (100 mm×2.1 mm, 1.8 μ m). The calibration was performed by the use of matrix-matched calibration standards. The results showed that there were good linear relationships for the four PAHs in the range of 2.4-40 μ g/L with correlation coefficients of 0.9990-0.9999. The limits of quantification (LOQs) ranged from 0.147 to 0.413 μ g/L, and the recoveries of the spiked samples ranged from 95.5% to 103.2%. The intra-day and inter-day precisions were in the ranges of 0.10%-1.69% and 2.48%-2.93% (n=5), respectively. The method has the characteristics of high sensitivity, low detection limit and good precision, and is suitable for rapid and accurate quantitative detection of the four PAHs in olive oil.