Rafiei Jam Mahdiye, Nezhadali Azizollah, Kaykhaii Massoud
Department of Chemistry, Payame Noor University, P.O. Box 19395-4697, 19569, Tehran, Iran.
Department of Process Engineering and Chemical Technology, Faculty of Chemistry, Gdańsk University of Technology, 80-233, Gdańsk, Poland.
BMC Chem. 2022 May 6;16(1):29. doi: 10.1186/s13065-022-00823-z.
4-Methylimidazole (4-MeI) or 4-methyl-1H-imidazole, a slightly yellowish solid with molecular formula CHN, is a heterocyclic compound which supposedly does not exist as a natural product and is formed when carbohydrates are heating with ammonium compounds. This compound is used in pharmaceuticals, agriculture and photography chemicals, dyes and pigments, and rubber manufacturing. In the present study, a simple and efficient sample preparation method designated gas flow headspace liquid phase microextraction (GF-HS-SDME) was employed for the extraction and preconcentration of 4-methylimidazole (4-MeI) from food and beverage samples, before its determination by gas chromatography-mass spectrometry.
To investigate the optimal conditions for the extraction process in GF-HS-SDME method, factors affecting extraction, including selection of extraction solvent, vial volume, extraction solvent ratio, position of extracting solvent, drop volume, sample volume, stirring speed, temperature, extraction time, sample pH, ionic strength of the sample solution and gas flow rate were optimized by utilizing both one-variable-at-a-time method and Plackett-Burman design. The investigation of protocol was carried out by using a standard solution containing 100.0 μg L of 4-MeI in deionized water.
In this study, a simple and green analytical method based on GF-HS-SDME was proposed for the extraction and preconcentration of 4-MeI from foodstuffs, followed by GC-MS determination. The main advantage of this method is its high preconcentration factor and fastness due to the application of an inert gas stream during microextraction.
4-甲基咪唑(4-MeI)或4-甲基-1H-咪唑,是一种分子式为CHN的微黄色固体,它是一种杂环化合物,一般认为不是天然产物,是碳水化合物与铵化合物加热时形成的。该化合物用于制药、农业、摄影化学品、染料和颜料以及橡胶制造。在本研究中,一种简单高效的样品制备方法——气流顶空液相微萃取(GF-HS-SDME)被用于从食品和饮料样品中萃取和预浓缩4-甲基咪唑(4-MeI),然后通过气相色谱-质谱联用仪进行测定。
为了研究GF-HS-SDME方法中萃取过程的最佳条件,通过单因素法和Plackett-Burman设计对影响萃取的因素进行了优化,这些因素包括萃取溶剂的选择、小瓶体积、萃取溶剂比例、萃取溶剂位置、液滴体积、样品体积、搅拌速度、温度、萃取时间、样品pH值、样品溶液的离子强度和气流速率。使用含有100.0μg/L 4-MeI的去离子水标准溶液对该方法进行了研究。
本研究提出了一种基于GF-HS-SDME的简单绿色分析方法,用于从食品中萃取和预浓缩4-MeI,随后进行GC-MS测定。该方法的主要优点是在微萃取过程中应用惰性气流,具有高预浓缩因子和快速性。