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基于 PDMS/离子液体海绵的固相萃取结合气相色谱-质谱法快速灵敏测定薰衣草中挥发性成分

Solid-phase extraction based on PDMS/ionic liquid sponge followed by gas chromatography-mass spectrometry for rapid and sensitive determination of volatile components in lavender.

机构信息

School of Chemical Engineering and Technology, Xinjiang University, Urumqi, China.

出版信息

Phytochem Anal. 2023 Mar;34(2):225-239. doi: 10.1002/pca.3199. Epub 2022 Dec 25.

Abstract

INTRODUCTION

Due to the complexity and the low concentrations of volatile components in aromatic plants, sample pretreatment is an important step in the whole analytical procedure.

OBJECTIVE

This study aimed to propose a novel, sensitive and fast approach to determine the volatile components in lavender.

METHODS

The 1-butyl-3-(propyltrimethoxysilane)imidazolium chloride ([BPtmsim]Cl) ionic liquid was introduced onto the surface of polydimethylsiloxane (PDMS) to prepare a novel PDMS/[BPtmsim]Cl sponge with large surface area, good sorption performance, and reusability. A solid-phase extraction method was developed based on PDMS/[BPtmsim]Cl sponge combined with gas chromatography-mass spectrometry (GC-MS).

RESULTS

The effects of the various experimental parameters on the extraction efficiency were investigated. The optimal conditions were [BPtmsim]Cl amount of 0.3 g, 1:4 as the mass ratio of PDMS/[BPtmsim]Cl to lavender sample, microwave power of 700 W, microwave time of 10 min, and n-hexane as the desorption solvent. The method validation results showed good linearity (10-800 μg/ml), high correlation coefficient (R  ≥ 0.9991), low limits of detection (1.73-2.50 ng/μl), and limits of quantification (4.10-5.11 ng/μl). The interday and intraday precision with relative standard deviation (RSD) values were below 1.93% and 4.71%, respectively. Under the optimal extraction conditions, 16 lavender samples from three different species were analysed and a total of 57 volatile compounds were identified. The correlation between different species of lavender and volatile components was explored using principal component analysis (PCA) and partial least squares-discriminant analysis (PLS-DA).

CONCLUSION

The results showed that PDMS/[BPtmsim]Cl extraction is a rapid, highly efficient, and sensitive technique for the determination of volatile components in complex plant samples.

摘要

简介

由于芳香植物中挥发性成分的复杂性和低浓度,样品前处理是整个分析过程中的重要步骤。

目的

本研究旨在提出一种新的、灵敏、快速的方法来测定薰衣草中的挥发性成分。

方法

将 1-丁基-3-(丙基三甲氧基硅烷)咪唑氯([BPtmsim]Cl)离子液体引入到聚二甲基硅氧烷(PDMS)表面,制备具有大表面积、良好吸附性能和可重复使用的新型 PDMS/[BPtmsim]Cl 海绵。基于 PDMS/[BPtmsim]Cl 海绵结合气相色谱-质谱联用(GC-MS)建立了固相萃取方法。

结果

考察了各种实验参数对萃取效率的影响。优化条件为[BPtmsim]Cl 用量 0.3 g,PDMS/[BPtmsim]Cl 与薰衣草样品的质量比为 1:4,微波功率 700 W,微波时间 10 min,正己烷为洗脱溶剂。方法验证结果表明,该方法具有良好的线性关系(10-800 μg/ml),高相关系数(R ≥ 0.9991),低检测限(1.73-2.50 ng/μl)和定量限(4.10-5.11 ng/μl)。日内和日间精密度的相对标准偏差(RSD)值分别低于 1.93%和 4.71%。在最佳提取条件下,分析了来自三个不同种的 16 个薰衣草样品,共鉴定出 57 种挥发性化合物。利用主成分分析(PCA)和偏最小二乘判别分析(PLS-DA)探讨了不同种薰衣草与挥发性成分的相关性。

结论

结果表明,PDMS/[BPtmsim]Cl 萃取是一种快速、高效、灵敏的技术,可用于测定复杂植物样品中的挥发性成分。

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