采用 SPE 与二维平面色谱法结合二极管阵列扫描密度法和 HPLC-二极管阵列检测器测定中草药提取物中的分析物。

Determination of analytes in medical herbs extracts by SPE coupled with two-dimensional planar chromatography in combination with diode array scanning densitometry and HPLC-diode array detector.

机构信息

Department of Physical Chemistry, Chair of Chemistry, Faculty of Pharmacy with Medical Analytics Division, Medical University of Lublin, Lublin, Poland.

出版信息

J Sep Sci. 2011 Jan;34(1):27-36. doi: 10.1002/jssc.201000582. Epub 2010 Nov 26.

DOI:10.1002/jssc.201000582

PMID:21171173

Abstract

The purpose of this study is to demonstrate an application of 2-D high-performance planar chromatography-diode array detector (DAD) and HPLC-DAD after solid-phase extraction (SPE) for identification and quantitative analysis of pesticides (isoproturon, aziprotryne, hexazinone, flufenoxuron, methabenzthiazuron, procymidone, and α-cypermethrin) in Melissa officinalis L. (Labiatae) samples. The procedure described for the determination of compounds is inexpensive and can be applied to routine analysis of analytes in medical herbs' samples after preliminary cleanup and concentration by SPE. Average recoveries on C18 SPE cartridges of pesticides eluted with 5 mL tetrahydrofuran by the proposed HPLC-DAD method, before and after 2-D-high-performance planar chromatography separation of analytes from M. officinalis L. samples spiked with pesticide at a concentration level of 10 μg/g in plant material are presented. Method validation parameters for the quantification of pesticides by the proposed HPLC-DAD after SPE method are also presented.

摘要

本研究旨在展示 2-D 高效平面色谱-二极管阵列检测器（DAD）和高效液相色谱-二极管阵列检测器（HPLC-DAD）在固相萃取（SPE）后的应用，用于鉴定和定量分析迷迭香（唇形科）样品中的农药（异丙隆、唑草酮、环嗪酮、氟虫脲、灭蝇胺、苯菌灵和α-氯氰菊酯）。用于测定化合物的程序价格低廉，可应用于通过 SPE 进行初步净化和浓缩后，对草药样品中的分析物进行常规分析。通过 HPLC-DAD 方法，用 5 mL 四氢呋喃洗脱 C18 SPE 小柱，对添加了 10 μg/g 植物材料中农药的迷迭香样品进行 2-D 高效平面色谱分离前后，提出了用提议的 HPLC-DAD 方法对农药进行 SPE 前和 SPE 后的平均回收率。还提出了通过 SPE 后 HPLC-DAD 方法对农药进行定量的方法验证参数。