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用液相色谱-电子电离-质谱法测定天然除虫菊酯。

Determination of natural pyrethrins by liquid chromatography-electron ionisation-mass spectrometry.

机构信息

University of Urbino, Urbino, Italy.

出版信息

Phytochem Anal. 2012 May-Jun;23(3):191-6. doi: 10.1002/pca.1342. Epub 2011 Jul 19.

DOI:10.1002/pca.1342
PMID:21774016
Abstract

INTRODUCTION

Pyrethrum extract is a mixture of six insecticidal compounds from the flower heads of Chrysanthemum cinerariaefolium L.. Since they only have low to moderate mammalian toxicity they can be used as natural insecticides in agriculture or to develop low cost and safe dermatological formulations. Because of the thermal instability of pyrethrins, analytical methods based on liquid chromatography (LC) are preferred over those based on gas chromatography (GC). A few applications using LC with mass spectrometry detection are presented in the literature. Current protocols for their characterisation by LC rely on the use of less sophisticated detectors such as UV detection.

OBJECTIVE

To develop the first liquid chromatography-electron ionisation-mass spectrometry (LC-EI-MS) method for pyrethrins detection and quantitation in pyrethrum extracts.

METHODOLOGY

A commercial pyrethrum extract and various samples of flower heads from C. cinerariaefolium L. were investigated using reversed-phase nano-liquid chromatography coupled to direct electron ionisation-mass spectrometry (nanoLC-direct EI-MS). The eluted compounds were identified through searches of the US National Institute of Standards and Technology (NIST) library, exploiting the direct EI capability to produce high quality EI mass spectra.

RESULTS

The method demonstrated satisfactory sensitivity (limit of detection (LOD) range: 0.04-0.38 mg/g), linearity (R² range: 0.9740-0.9983) and precision (RSD% range: 4-13%) for the quantitation of the natural pyrethrins in extracts from C. cinerariaefolium L.

CONCLUSION

The nanoLC-direct EI-MS technique can be a useful tool for the detection of pyrethrins.

摘要

简介

除虫菊提取物是从菊科植物除虫菊花头中提取的六种杀虫化合物的混合物。由于它们对哺乳动物的毒性低至中等,因此可以在农业中用作天然杀虫剂,或开发低成本和安全的皮肤科制剂。由于除虫菊素的热不稳定性,基于液相色谱(LC)的分析方法优于基于气相色谱(GC)的方法。文献中介绍了一些使用 LC 与质谱检测联用的应用。目前,LC 用于其特征描述的方案依赖于使用更简单的检测器,如紫外检测。

目的

开发首个用于除虫菊提取物中除虫菊素检测和定量的液相色谱-电子电离-质谱(LC-EI-MS)方法。

方法

使用反相纳米液相色谱与直接电子电离-质谱(nanoLC-direct EI-MS)联用,对商业除虫菊提取物和菊科植物 C. cinerariaefolium L. 的各种花头样本进行了研究。通过对美国国家标准与技术研究院(NIST)库进行搜索,利用直接 EI 产生高质量 EI 质谱的能力,对洗脱化合物进行了鉴定。

结果

该方法对从 C. cinerariaefolium L. 提取物中定量天然除虫菊素具有令人满意的灵敏度(检测限范围:0.04-0.38 mg/g)、线性(R²范围:0.9740-0.9983)和精密度(RSD%范围:4-13%)。

结论

nanoLC-direct EI-MS 技术可作为检测除虫菊素的有用工具。

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