通过固相萃取-超临界流体萃取和气相色谱-质谱联用技术检测尿液中的β受体阻滞剂。

Detection of beta-blockers in urine by solid-phase extraction-supercritical fluid extraction and gas chromatography-mass spectrometry.

作者信息

Hartonen K, Riekkola M L

机构信息

Department of Chemistry, University of Helsinki, Finland.

出版信息

J Chromatogr B Biomed Appl. 1996 Feb 9;676(1):45-52. doi: 10.1016/0378-4347(95)00373-8.

DOI:10.1016/0378-4347(95)00373-8

PMID:8852043

Abstract

The most convenient way to perform supercritical fluid extraction (SFE) of liquid sample matrices is to combine it with solid-phase extraction (SPE). beta-Blockers from urine were collected on an Empore disc, which was then placed into an extraction cell for derivatization and SFE. SPE recovery was best at pH 10. Effects of temperature, pressure and volume of pyridine on the acetylation and SFE processes were studied. Without acetylation the beta-blockers were not significantly soluble in CO2. SFE temperatures of 70 degree C and 150 degree C together with 200 microliters of acetic anhydride and 400 microliters pyridine gave the best results. With the SPE-SFE-GC-MS method developed here, beta-blockers like oxprenolol, metoprolol and propranolol could easily be detected in urine samples, and the limit of detection (LOD) for these compounds was found to be 20 ng/ml, 30 ng/ml and 40 ng/ml, respectively.

摘要

对液体样品基质进行超临界流体萃取（SFE）最便捷的方法是将其与固相萃取（SPE）相结合。尿液中的β-受体阻滞剂收集在Empore盘上，然后将其放入萃取池中进行衍生化和SFE。SPE回收率在pH 10时最佳。研究了温度、压力和吡啶体积对乙酰化和SFE过程的影响。未进行乙酰化时，β-受体阻滞剂在CO2中溶解度不显著。70℃和150℃的SFE温度以及200微升乙酸酐和400微升吡啶效果最佳。采用此处开发的SPE-SFE-GC-MS方法，可轻松检测尿液样本中的氧烯洛尔、美托洛尔和普萘洛尔等β-受体阻滞剂，这些化合物的检测限分别为20 ng/ml、30 ng/ml和40 ng/ml。