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目的建立采用超高效液相色谱(UPLC)-荧光检测器(FLR)同时快速检测植物油中15种多环芳烃的方法。方法采用乙腈∶丙酮(1∶1)混合溶剂提取,先后使用Waters的Oasis HLB和Sep-Pak Florsil小柱净化,Waters PAH C18色谱柱(4.6mm×50 mm,3μm)分离,甲醇、乙腈和水进行梯度洗脱,柱温35℃,流速0.80 ml/min,进样量10μl;荧光检测器采用程序定时控制荧光检测波长变化,外标法定量。结果 15种多环芳烃9 min内完全分离,在2.0~200.0μg/L范围内,峰面积和质量浓度的线性关系良好(r≥0.9990),以高、中、低浓度(10、50和100μg/kg)作为不同的添加水平,平均加标回收率为75.8%~96.4%,RSD为3.42%~8.03%(n=5),检出限为0.025~0.8μg/kg,定量限为0.08,3.0μg/kg。结论该方法操作方便、分离效果好、线性范围宽,能满足植物油中15种多环芳烃的检测要求。
Objective To establish a rapid and simultaneous method for the simultaneous determination of 15 polycyclic aromatic hydrocarbons (PAHs) in vegetable oils by ultra performance liquid chromatography (UPLC) - fluorescence detector (FLR). The method was extracted with a mixed solvent of acetonitrile and acetone (1: 1), then purified on a Waters Oasis HLB and Sep-Pak Florsil cartridges, separated on a Waters PAH C18 column (4.6 mm × 50 mm, 3 μm) Gradient elution, the column temperature 35 ℃, the flow rate of 0.80 ml / min, the injection volume 10μl; fluorescence detector using program timing control fluorescence detection wavelength change, external standard method. Results 15 polycyclic aromatic hydrocarbons (PAHs) were completely separated within 9 min. The linear relationship between peak area and mass concentration was good (r ≥ 0.9990) in the range of 2.0 ~ 200.0 μg / L. / kg) as different addition levels, the average recovery was 75.8% ~ 96.4%, RSD was 3.42% ~ 8.03% (n = 5), the detection limit was 0.025 ~ 0.8μg / kg, the limit of quantification was 0.08, 3.0 μg / kg. Conclusion The method is easy to operate with good separation effect and wide linear range. It can meet the detection requirements of 15 kinds of polycyclic aromatic hydrocarbons in vegetable oil.