Cloud‐Point Extraction and Reversed‐Phase High‐Performance Liquid Chromatography for the Determination of Synthetic Phenolic Antioxidants in Edible Oils

Abstract

A cloud-point extraction (CPE) method using Triton X-114 (TX-114) nonionic surfactant was developed for the extraction and preconcentration of propyl gallate (PG), tertiary butyl hydroquinone (TBHQ), butylated hydroxyanisole (BHA), and butylated hydroxytoluene (BHT) from edible oils. The optimum conditions of CPE were 2.5% (v/v) TX-114, 0.5% (w/v) NaCl and 40 min equilibration time at 50 °C. The surfactant-rich phase was then analyzed by reversed-phase high-performance liquid chromatography with ultraviolet detection at 280 nm, using a gradient mobile phase consisting of methanol and 1.5% (v/v) acetic acid. Under the studied conditions, 4 synthetic phenolic antioxidants (SPAs) were successfully separated within 24 min. The limits of detection (LOD) were 1.9 ng mL(-1) for PG, 11 ng mL(-1) for TBHQ, 2.3 ng mL(-1) for BHA, and 5.9 ng mL(-1) for BHT. Recoveries of the SPAs spiked into edible oil were in the range 81% to 88%. The CPE method was shown to be potentially useful for the preconcentration of the target analytes, with a preconcentration factor of 14. Moreover, the method is simple, has high sensitivity, consumes much less solvent than traditional methods, and is environment-friendly. Practical Application: The method established in this article uses less organic solvent to extract SPAs from edible oils; it is simple, highly sensitive and results in no pollution to the environment.

Determination of synthetic phenolic antioxidants in soft drinks by stir-bar sorptive extraction coupled to gas chromatography-mass spectrometry

“…The determination of phenolic antioxidants has been accomplished using LC coupled with different detectors, such as ultraviolet (UV) light (Rafecas et al 1998;Maziero et al 2001;Saad et al 2007;Akkbik et al 2011;Chen et al 2011Chen et al , 2013Biparva et al 2012;Wang et al 2012;Barbosa-Pereira et al 2013;Çabuk & Köktürk 2013) or MS (Tsuji et al 2005;Lee et al 2006;Xiu-Qin et al 2009;Barbosa-Pereira et al 2013 Jamshidian et al 2013). GC (Yang et al 2002(Yang et al , 2010Suh et al 2005;Tsuji et al 2005;Guo et al 2006;Ding & Zou 2012;Rodil et al 2012;Tranchida et al 2013) has also been used for the determination of these compounds, MS being the most commonly used detector (Tsuji et al 2005;Guo et al 2006;Yang et al 2010;Ding & Zou 2012;Rodil et al 2012;Tranchida et al 2013).…”

“…Taking into account the low expected concentration of these antioxidants in soft drinks, a pre-concentration step is required. Classical enrichment methods, like SPE (Tsuji et al 2005;Rodil et al 2012) or liquid-liquid extraction (LLE) (Xiu-Qin et al 2009) have been proposed, but in recent years new micro-extraction procedures, like solidphase micro-extraction (SPME) (Yang et al 2010) and different modes of liquid-liquid micro-extraction (LLME) (Chen et al 2011Biparva et al 2012;Çabuk & Köktürk 2013), have been applied for the preconcentration of phenolic antioxidants from different sample matrices. These procedures, which are usually less time-consuming and require lower volumes of organic solvents than classical techniques, are clean, selective, rapid and efficient.…”

Vortex-Assisted Deep Eutectic Solvent-Based Liquid-Liquid Microextraction for the Analysis of Alkyl Gallates in Vegetable Oils

“…Generally, the allowed amounts of SAs in food range from 100 to 200 mg kg -1 in European Union, either singly or in combination. 5 The determination of alkyl gallates in foodstuffs has been accomplished using specific electrochemical sen-sors [6][7][8] and different separation techniques such as high-performance liquid chromatography (HPLC), 5,[9][10][11][12] micellar electrokinetic capillary chromatography 13,14 and capillary electrophoresis. 15,16 Electrochemical methods may offer relatively low operational costs and faster analysis.…”

“…18,19 However, a pretreatment step for sample enrichment and cleanup is always desirable prior to any chromatographic analysis due to the complexity of the sample matrix. Recently, some novel microextraction procedures, such as cloud-point extraction (CPE) 10 and dispersive liquid-liquid microextraction (DLLME) 5,20 have also been devel-…”

Utility of 4‐Chloro‐7‐Nitrobenzofurazan for the Spectrofluorimetric Determination of Butylated Hydroxyanisole and Propyl Gallate in Foodstuffs

“…High‐performance liquid chromatography (HPLC) has been the most widely used method for the determination of synthetic antioxidants. Reversed‐phase HPLC provides high selectivity for the separation of synthetic antioxidants under mild chromatographic conditions (Ruiz and others 1999; Aparicio and others 2000; Chen and others 2011), thin‐layer chromatography (Sin and others 2006), gas chromatography (Min and Schweizer 2006), gas liquid chromatography (Greenberg and others 2006), and micellar electrokinetic capillary chromatography analytical methods have also been used for SPA analysis (Wang and others 2010).…”