Triple Quadrupole Mass Spectrometry with Liquid Chromatography and Dispersive Liquid-Liquid Microextraction for the Dete
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Triple Quadrupole Mass Spectrometry with Liquid Chromatography and Dispersive Liquid-Liquid Microextraction for the Determination of Monoterpenes in Alcoholic Drinks Ainhoa Oller-Ruiz 1 & Pilar Viñas 1 & Natalia Campillo 1 & José Fenoll 2 & Manuel Hernández-Córdoba 1
Received: 17 February 2017 / Accepted: 10 May 2017 # Springer Science+Business Media New York 2017
Abstract Five monoterpenes (linalool, geraniol, eugenol, carvacrol, and thymol) were directly preconcentrated from alcoholic drinks with no previous sample treatment step using a miniaturized technique based on dispersive liquidliquid microextraction. Chloroform (300 μL) was rapidly injected into 8 mL of sample, while the addition of a disperser solvent was obviated because of the ethanol content of the alcoholic beverages. The enriched phase was evaporated, reconstituted in 50 μL water, and analyzed by reversed phase liquid chromatography with a mobile phase consisting of 25% acetonitrile (0.1% formic acid) and 75% water (0.1% formic acid) and tandem mass spectrometry with a triple quadrupole in the selected reaction monitoring mode. The matrix effect was evaluated, and quantification by the standard additions method is recommended. Limits of detection ranged from 0.003 to 1.5 ng mL−1, depending on the compound and the matrix. Enrichment factors of between 12 and 88 were obtained. The method was validated through recovery tests, finding values in the 76–128% range. The intraday precision was lower than 20% in terms of relative standard deviation. Different types of alcoholic drinks were analyzed, monoterpenes being detected at concentrations from 0.4 to 627 ng mL−1.
* Manuel Hernández-Córdoba [email protected] 1
Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence BCampus Mare Nostrum^, University of Murcia, 30100 Murcia, Spain
2
Department of Food Quality and Warranty, IMIDA, c/Mayor s/n, La Alberca, 30150 Murcia, Spain
Keywords Dispersive liquid-liquid microextraction (DLLME) . Liquid chromatography (LC) . Triple quadrupole mass spectrometry (QqQ-MS2) . Monoterpenes . Alcoholic drinks
Introduction Monoterpenes are highly volatile isoprene-derived chemical compounds found at high concentrations in essential oils from different kinds of plants including lavender, citronella, rose, citrus, mint, thyme, oregano, bay leaf, cinnamon, cloves, and nutmeg. Their beneficial effects include antimicrobial, antifungal, anti-inflammatory, antibacterial, and anticancer activities (Mirón et al. 2014). Because of their characteristics and volatility, terpenes are frequently used in the cosmetic and food industries as they are important as aroma components. Although no toxic effects have been reported except when they are present at very high concentration levels, their determination is of great importance for evaluating both the quality and organoleptic characteristics of food and beverages. In this study, different kinds of alcoholic drink, which are very complex samples containing terpenes, alcohols, ketones, este
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