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Nano and rapid resolution liquid chromatography-electrospray ionization-time of flight mass spectrometry to identify and quantify phenolic compounds in olive oil

机译:纳米级和快速分离液相色谱-电喷雾电离-飞行时间质谱法鉴定和定量橄榄油中的酚类化合物

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摘要

The applicability of nanoLC-ESI-TOF MS for the analysis of phenolic compounds in olive oil was studied and compared with a HPLC method. After the injection, the compounds were focused on a short capillary trapping column (100 μm id, effective length 20mm, 5 μm particle size) and then nanoLC analysis was carried out in a fused silica capillary column (75 μm id, effective length 10 μm, 3 μm particle size) packed with C18 stationary phase. The mobile phase was a mixture of water +0.5% acetic acid and ACN eluting at 300 nL/min in a gradient mode. Phenolic compounds from different families were identified and quantified. The quality parameters of the nanoLC method (linearity, LODs and LOQs, repeatability) were evaluated and compared with those obtained with HPLC. The new methodology presents better sensitivity (reaching LOD values below 1 ppb) with less consumption of mobile phases, but worse repeatability, especially inter-day repeatability, resulting in more difficulties to get highly accurate quantification. The results described in this article open up the application fields of this technique to cover a larger variety of compounds and its advantages will make it especially useful for the analysis of samples containing low concentration of phenolic compounds, as for instance, in biological samples.
机译:研究了nanoLC-ESI-TOF MS在分析橄榄油中酚类化合物中的适用性,并与HPLC方法进行了比较。进样后,将化合物聚焦在短毛细管捕集柱(内径100μm,有效长度20mm,粒径5μm)上,然后在熔融石英毛细管柱(内径75μm,有效长度10μm)中进行nanoLC分析。 (粒径为3μm)填充有C18固定相。流动相是水+ 0.5%乙酸和ACN的混合物,以300 nL / min的梯度洗脱。鉴定和量化了来自不同家族的酚类化合物。评估了nanoLC方法的质量参数(线性,LOD和LOQ,重复性),并将其与HPLC进行了比较。新方法具有更高的灵敏度(达到LOD值低于1 ppb),流动相消耗更少,但可重复性(尤其是日间重复性)更差,导致获得高度准确定量的难度更大。本文中描述的结果开拓了该技术的应用领域,以涵盖更多种类的化合物,其优点将使其特别适用于分析含低浓度酚类化合物的样品,例如生物样品。

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