迈向用于生物流体中药物代谢物痕量分析的无干扰高效液相色谱-表面增强拉曼光谱法。
Towards interference free HPLC-SERS for the trace analysis of drug metabolites in biological fluids.
作者信息
Hassanain Waleed A, Izake Emad L, Sivanesan Arumugam, Ayoko Godwin A
机构信息
School of Chemistry, Physics and Mechanical Engineering, Queensland University of Technology, 2 George St, Brisbane QLD 4000, Australia.
School of Chemistry, Physics and Mechanical Engineering, Queensland University of Technology, 2 George St, Brisbane QLD 4000, Australia.
出版信息
J Pharm Biomed Anal. 2017 Mar 20;136:38-43. doi: 10.1016/j.jpba.2016.12.019. Epub 2016 Dec 23.
Sofosbuvir metabolite, 2'-deoxy-2'-fluoro-2'-C-methyluridine (PSI-6206) was studied for the first time by surface enhanced Raman spectroscopy (SERS) using the paper-based SERS substrate. The quantification limit of PSI-6206 by SERS was found to be 13ngL (R value=0.959, RSD=5.23%). For the structural and quantitative analysis of PSI-6206 in blood plasma, an interference-free HPLC-SERS method was developed and compared to HPLC-DAD and HPLC-MS methods. The SERS quantification of the drug by the paper substrate was 4 orders of magnitude more sensitive than that by the diode array detector. In addition, the SERS detection provided unique structural identification of the drug in blood plasma, similar to Mass spectroscopy detector. Due to the disposable nature of the SERS substrate, the new method does not suffer from the known "memory effect" which is known to lead to false positive identification in traditional HPLC-SERS methods. Therefore, the presented HPLC-paper SERS platform holds great potential for the sensitive and cost effective determination of drugs and their metabolites in biological fluids.
首次使用基于纸张的表面增强拉曼光谱（SERS）底物，通过表面增强拉曼光谱（SERS）对索磷布韦代谢物2'-脱氧-2'-氟-2'-C-甲基尿苷（PSI-6206）进行了研究。通过SERS测定PSI-6206的定量限为13ng/L（R值 = 0.959，相对标准偏差 = 5.23%）。为了对血浆中的PSI-6206进行结构和定量分析，开发了一种无干扰的高效液相色谱 - 表面增强拉曼光谱（HPLC-SERS）方法，并与高效液相色谱 - 二极管阵列检测器（HPLC-DAD）和高效液相色谱 - 质谱（HPLC-MS）方法进行了比较。纸质底物对该药物的SERS定量比二极管阵列检测器灵敏4个数量级。此外，SERS检测提供了血浆中该药物独特的结构鉴定，类似于质谱检测器。由于SERS底物的一次性使用性质，新方法不存在传统HPLC-SERS方法中已知的会导致假阳性鉴定的“记忆效应”。因此，所提出的HPLC-纸质SERS平台在灵敏且经济高效地测定生物流体中的药物及其代谢物方面具有巨大潜力。
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