scholarly journals New Sample Preparation Method for Honey Volatiles Fingerprinting Based on Dehydration Homogeneous Liquid–Liquid Extraction (DHLLE)

Molecules ◽  
2018 ◽  
Vol 23 (7) ◽  
pp. 1769 ◽  
Author(s):  
Piotr Kuś ◽  
Igor Jerković
Keyword(s):  
Sample Preparation ◽  
Preparation Method ◽  
Solvent Polarity ◽  
Liquid Extraction ◽  
Sample Preparation Method ◽  
Preparation Methods ◽  
Homogeneous Liquid ◽  
Liquid Liquid Extraction ◽  
Relative Standard ◽  
Honey Solution

Qualitative chemical fingerprinting of the honey volatiles by gas chromatography and mass spectrometry (GC-MS) has been an efficient authentication tool that allowed for the classification of the honey botanical origin (strongly related to its medicinal and market value). However, the usage of current sample preparation methods is limited by selectivity of the volatiles extraction from the honey matrix and requires significant solvent volume. Therefore, a new sample preparation method based on dehydrating homogeneous liquid–liquid extraction (DHLLE) involving reduced solvent usage was developed for screening volatiles and semi-volatiles from the honey. The effective extraction was achieved by implementing a miscible liquid extraction system (aqueous honey solution/isopropanol) followed by separation through dehydration with MgSO4 and purification by a solvent polarity change and washing. The method was evaluated by estimating accuracy and precision. The DHLLE method showed satisfactory recoveries (75.2 to 93.5%) for typical honey volatiles: linalool, borneol, terpinen-4-ol, α-terpineol, p-anisaldehyde, eugenol, and vanillin. It also showed superior repeatability with percent relative standard deviation (RSD%) 0.8–8.9%. For benzyl alcohol, methyl syringate, and caffeine, the recoveries were 54.3 to 63.9% and 67.3 to 77.7% at lower and higher spiking levels, respectively. Applied to unifloral apple honey, the DHLLE method allowed for the identification of 40 compounds including terpenes, hydrocarbons, phenylpropanoids, and other benzene derivatives, which makes it suitable for fingerprinting and chemical marker screening. The obtained results were comparable or better than those obtained with ultrasonic extraction with dichloromethane.

scholarly journals Application of the Dehydration Homogeneous Liquid–Liquid Extraction (DHLLE) Sample Preparation Method for Fingerprinting of Honey Volatiles

Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2277
Author(s):  
Piotr M. Kuś ◽  
Igor Jerković
Keyword(s):  
Carboxylic Acid ◽  
Sample Preparation ◽  
Preparation Method ◽  
Liquid Extraction ◽  
Sample Preparation Method ◽  
Phenyllactic Acid ◽  
Homogeneous Liquid ◽  
Liquid Liquid Extraction ◽  
Wide Range ◽  
Chemical Groups

Recently, we proposed a new sample preparation method involving reduced solvent and sample usage, based on dehydration homogeneous liquid–liquid extraction (DHLLE) for the screening of volatiles and semi-volatiles from honey. In the present research, the method was applied to a wide range of honeys (21 different representative unifloral samples) to determine its suitability for detecting characteristic honey compounds from different chemical classes. GC-FID/MS disclosed 130 compounds from different structural and chemical groups. The DHLLE method allowed the extraction and identification of a wide range of previously reported specific and nonspecific marker compounds belonging to different chemical groups (including monoterpenes, norisoprenoids, benzene derivatives, or nitrogen compounds). For example, DHLLE allowed the detection of cornflower honey chemical markers: 3-oxo-retro-α-ionols, 3,4-dihydro-3-oxoedulan, phenyllactic acid; coffee honey markers: theobromine and caffeine; linden honey markers: 4-isopropenylcyclohexa-1,3-diene-1-carboxylic acid and 4-(2-hydroxy-2-propanyl)cyclohexa-1,3-diene-1-carboxylic acid, as well as furan derivatives from buckwheat honey. The obtained results were comparable with the previously reported data on markers of various honey varieties. Considering the application of much lower volumes of very common reagents, DHLLE may provide economical and ecological advantages as an alternative sample preparation method for routine purposes.

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

Molecules ◽  
2019 ◽  
Vol 24 (15) ◽  
pp. 2761 ◽  
Author(s):  
Wenbin Chen ◽  
Siyuan Wu ◽  
Jianing Zhang ◽  
Fengjie Yu ◽  
Jianbo Hou ◽  
...  
Keyword(s):  
Phase Separation ◽  
Sample Preparation ◽  
Preparation Method ◽  
Liquid Extraction ◽  
Subzero Temperature ◽  
Water Mixture ◽  
Sample Preparation Method ◽  
Liquid Liquid Extraction ◽  
Neonicotinoid Pesticides

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.

Salting-out-assisted liquid–liquid extraction of 5-hydroxymethylfurfural from honey and the determination of 5-hydroxymethylfurfural by high-performance liquid chromatography

2019 ◽  
Vol 11 (37) ◽  
pp. 4835-4841 ◽  
Author(s):  
Wenbin Chen ◽  
Siyuan Wu ◽  
Jianing Zhang ◽  
Fengjie Yu ◽  
Xiaoqing Miao ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
High Performance ◽  
Preparation Method ◽  
Liquid Extraction ◽  
Sample Preparation Method ◽  
Salting Out ◽  
Liquid Liquid Extraction

A simple, rapid, and effective sample preparation method was developed for the recovery of 5-hydroxymethylfurfural from honey samples with negligible co-extracted sugars.

scholarly journals Homogeneous Liquid-Liquid Extraction Method for Selective Separation and Preconcentration of Trace Amounts of Palladium

2009 ◽  
Vol 6 (4) ◽  
pp. 1077-1084 ◽  
Author(s):  
Mohammad Reza Jamali ◽  
Yaghoub Assadi ◽  
Reyhaneh Rahnama Kozani ◽  
Farzaneh Shemirani
Keyword(s):  
Extraction Method ◽  
Limit Of Detection ◽  
Liquid Extraction ◽  
Selective Separation ◽  
Complexing Agent ◽  
Homogeneous Liquid ◽  
Liquid Liquid Extraction ◽  
Relative Standard ◽  
Separation And Preconcentration ◽  
Ternary Component System

A simple and effective homogeneous liquid-liquid extraction method for selective separation, preconcentration and spectrophotometric determination of palladium(II) ion was developed by using a ternary component system (water / tetrabutylammonium ion (TBA+) / chloroform). The phase separation phenomenon occurred by an ion–pair formation of TBA+and perchlorate ion. Thio-Michler’s ketone (TMK), 4, 4ˊ-bis (dimethylamino) thiobenzophenone, was used as a complexing agent. After optimization of complexation and extraction conditions ([TMK]=5.0x10-2mol L-1, [TBA+] = 2.0×10-2mol L-1, [CHCl3] = 60.0 µL, [ClO4-] = 2.5×10-2mol L-1and pH= 3.0), a preconcentration factor 10 was obtained for 10 mL of sample. The analytical curve was linear in the range of 2-100 ng mL-1and the limit of detection was 0.4 ng mL-1. The relative standard deviation was 3.2% (n=10). Accuracy and application of the method was estimated by using test samples of natural and synthetic water spiked with different amounts of palladium(II) ion. The method is very simple and inexpensive.

Study on Sample Preparation Method of DEM

2013 ◽  
Vol 671-674 ◽  
pp. 333-336
Author(s):  
Yang Liu ◽  
Xian De Zhu ◽  
Chen Ye Wan
Keyword(s):  
Sample Preparation ◽  
Discrete Element Method ◽  
Preparation Method ◽  
Descent Method ◽  
Mechanical Parameters ◽  
Sample Preparation Method ◽  
Preparation Methods ◽  
Dem Model ◽  
Compaction Method ◽  
Sample Preparation Methods

Three numerical sample preparation methods, namely, radius expand method, hierarchical compaction method and gravity descent method, were studied using discrete element method (DEM) to simulate the actual sample. The processes of these three methods were described in details and the differences of these three methods were discussed. The impacts of mechanical parameters in DEM model on the numerical results were analyzed.

scholarly journals Sample preparation method to improve the efficiency of high-throughput single-molecule force spectroscopy

2019 ◽  
Vol 5 (4) ◽  
pp. 176-183 ◽  
Author(s):  
Lei Jin ◽  
Li Kou ◽  
Yanan Zeng ◽  
Chunguang Hu ◽  
Xiaodong Hu
Keyword(s):  
Sample Preparation ◽  
High Throughput ◽  
Single Molecule ◽  
Preparation Method ◽  
Force Spectroscopy ◽  
Experimental Result ◽  
Sample Preparation Method ◽  
Dna Stretching ◽  
Single Molecule Force Spectroscopy ◽  
Preparation Methods

Abstract Inefficient sample preparation methods hinder the performance of high-throughput single-molecule force spectroscopy (H-SMFS) for viscous damping among reactants and unstable linkage. Here, we demonstrated a sample preparation method for H-SMFS systems to achieve a higher ratio of effective target molecules per sample cell by gas-phase silanization and reactant hydrophobization. Digital holographic centrifugal force microscopy (DH-CFM) was used to verify its performance. The experimental result indicated that the DNA stretching success ratio was improved from 0.89% to 13.5%. This enhanced efficiency preparation method has potential application for force-based DNA stretching experiments and other modifying procedures.

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