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[高效液相色谱法定性定量测定唾液中的咖啡因]

[Qualitative and quantitative determination of caffeine in saliva by high performance liquid chromatography].

作者信息

Napierała Marta, Florek Ewa

出版信息

Przegl Lek. 2016;73(10):777-80.

Abstract

The European Union drew attention to the increased consumption and the reports of adverse reactions to caffeine in recent years. The EU Commission in Regulation No. 536/2013 dated 11 June 2013 expressed concern about the caffeine content in the products. It is important to develop a simple and accurate methods for determining the level of caffeine in the biological material for accurate exposure assessment, as well as in the caffeinated products. The use of saliva as a diagnostic material is painless, non-invasive and does not require the participation of professional medical personnel. The compounds identified in saliva showed relatively high durability. The developed method for the determination of caffeine by high performance liquid chromatography with diode array detection (HPLC-DAD) after extraction of caffeine from saliva by solid phase extraction (SPE) is characterized by the linearity in the concentration range 50 - 2000 ng/mL. This method have low detection (12 ng/mL) and quantification (40 ng/mL) limits and high intra-day (4.87% for low concentration and 2.10% for high concentration) and inter-day (5.84% for low concentration and 2.43% for high concentration) repeatability.

摘要

近年来,欧盟注意到咖啡因的消费量有所增加以及有关其不良反应的报告。欧盟委员会在2013年6月11日发布的第536/2013号法规中对产品中的咖啡因含量表示关切。为了进行准确的暴露评估,开发一种简单而准确的方法来测定生物材料以及含咖啡因产品中的咖啡因含量非常重要。使用唾液作为诊断材料无痛、无创,且无需专业医务人员参与。在唾液中鉴定出的化合物显示出相对较高的稳定性。所开发的通过固相萃取(SPE)从唾液中提取咖啡因后,采用高效液相色谱-二极管阵列检测(HPLC-DAD)测定咖啡因的方法,其浓度范围在50 - 2000 ng/mL时具有线性特征。该方法具有低检测限(12 ng/mL)和定量限(40 ng/mL),日内(低浓度为4.87%,高浓度为2.10%)和日间(低浓度为5.84%,高浓度为2.43%)重复性高。

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