Matrix-Induced Sugaring-Out: A Simple and Rapid Sample Preparation Method for the Determination of Neonicotinoid Pesticides in Honey

Abstract

In the present work, we developed a simple and rapid sample preparation method for the determination of neonicotinoid pesticides in honey based on the matrix-induced sugaring-out. Since there is a high concentration of sugars in the honey matrix, the honey samples were mixed directly with acetonitrile (ACN)-water mixture to trigger the phase separation. Analytes were extracted into the upper ACN phase without additional phase separation agents and injected into the HPLC system for the analysis. Parameters of this matrix-induced sugaring-out method were systematically investigated. The optimal protocol involves 2 g honey mixed with 4 mL ACN-water mixture (v/v, 60:40). In addition, this simple sample preparation method was compared with two other ACN-water-based homogenous liquid-liquid extraction methods, including salting-out assisted liquid-liquid extraction and subzero-temperature assisted liquid-liquid extraction. The present method was fully validated, the obtained limits of detection (LODs) and limits of quantification (LOQs) were from 21 to 27 and 70 to 90 μg/kg, respectively. Average recoveries at three spiked levels were in the range of 91.49% to 97.73%. Precision expressed as relative standard deviations (RSDs) in the inter-day and intra-day analysis were all lower than 5%. Finally, the developed method was applied for the analysis of eight honey samples, results showed that none of the target neonicotinoid residues were detected.

Miniaturized Salting-Out Assisted Liquid-Liquid Extraction Combined with Disposable Pipette Extraction for Fast Sample Preparation of Neonicotinoid Pesticides in Bee Pollen

“…The final cleaned-up solution was separated in C18 reversed-phase HPLC with gradient elution. Target neonicotinoid pesticides were quantified by an inner standard based on our previous report [42]. The diode array detector (DAD) was used for the detection of pesticides, and a wavelength of 254 nm was applied for the quantification.…”

Matrix‐induced sugaring‐out liquid‐liquid microextraction coupled with high‐performance liquid chromatography for the determination of organophosphorus pesticides in fruit jams

“…Another advantage of ACN, associated with being the most popular mobile phase in LC, is that its final extract can be directly analyzed [7]. The SULLME has been used for extracting analytes of varied polarity, e.g., drugs [9,[11][12][13], phenolic compounds [10], bioactive constituents [14,15], bisphenols [16], sulfonamides [17], and pesticides [18][19][20] from biological and/or food matrices. Glucose is most often preferred as a sugaring-out reagent, since it is cheap, easily available and efficient, and produces a less viscous solution [12].…”

Dispersive Membrane Microextraction of Substituted Phenols from Honey Samples and a Brief Outlook on Its Sustainability Using Analytical Eco-Scale and Analytical GREEnness Metric Approach

“…Recent reporting has indicated a worrying trend in the detection of these polar pollutants in everyday food items such as honey [ 12 , 13 , 14 ]. It is feared that due to the substituted phenols’ high resistance to biodegradation, they continue to retain their presence in food sources such as honey [ 12 , 22 ]. Researchers have propounded that the phenols could be sourced from the use of pesticides and herbicides in plants from which they are consequently transported by nectar-collecting traveling bees or via treated wooden beehives [ 13 , 14 ].…”

“…This study focuses on the use of a recently developed method [ 23 ], dispersive membrane microextraction (DMME), using sporopollenin–methylimidazolium-based mixed matrix membrane (Sp–MIM-MMM) alongside high-performance liquid chromatography (HPLC) to determine the presence of chloro- and nitro-substituted phenolsin honey samples procured from commercial and natural sources. DMME is an extension of DSPME where the Sp–MIM-MMM acts as a solid-phase adsorbent and has been reported to overcome the sample matrix effect quite successfully to determine the presence of the substituted phenols [ 22 ]. Following this, the sustainability of the DMME–HPLC method was also evaluated using the Analytical Eco-Scale (AES) [ 24 ] and the Analytical GREEnness Metric (AGREE) [ 25 ] approach.…”