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

Molecules ◽  
2020 ◽  
Vol 25 (23) ◽  
pp. 5703
Author(s):  
Xijuan Tu ◽  
Wenbin Chen

As the main source of nutrients for the important pollinator honeybee, bee pollen is crucial for the health of the honeybee and the agro-ecosystem. In the present study, a new sample preparation procedure has been developed for the determination of neonicotinoid pesticides in bee pollen. The neonicotinoid pesticides were extracted using miniaturized salting-out assisted liquid-liquid extraction (mini-SALLE), followed by disposable pipette extraction (DPX) for the clean-up of analytes. Effects of DPX parameters on the clean-up performance were systematically investigated, including sorbent types (PSA, C18, and silica gel), mass of sorbent, loading modes, and elution conditions. In addition, the clean-up effect of classical dispersive solid-phase extraction (d-SPE) was compared with that of the DPX method. Results indicated that PSA-based DPX showed excellent clean-up ability for the high performance liquid chromatography (HPLC) analysis of neonicotinoid pesticides in bee pollen. The proposed DPX method was fully validated and demonstrated to provide the advantage of simple and rapid clean-up with low consumption of solvent. This is the first report of DPX method applied in bee pollen matrix, and would be valuable for the development of a fast sample preparation method for this challenging and important matrix.

2019 ◽  
Vol 11 (37) ◽  
pp. 4835-4841 ◽  
Author(s):  
Wenbin Chen ◽  
Siyuan Wu ◽  
Jianing Zhang ◽  
Fengjie Yu ◽  
Xiaoqing Miao ◽  
...  

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


Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2350
Author(s):  
Jianing Zhang ◽  
Fengjie Yu ◽  
Yunmin Tao ◽  
Chunping Du ◽  
Wenchao Yang ◽  
...  

In the present work, a novel sample preparation method, micro salting-out assisted matrix solid-phase dispersion (μ-SOA-MSPD), was developed for the determination of bisphenol A (BPA) and bisphenol B (BPB) contaminants in bee pollen. The proposed method was designed to combine two classical sample preparation methodologies, matrix solid-phase dispersion (MSPD) and homogenous liquid-liquid extraction (HLLE), to simplify and speed-up the preparation process. Parameters of μ-SOA-MSPD were systematically investigated, and results indicated the significant effect of salt and ACN-H2O extractant on the signal response of analytes. In addition, excellent clean-up ability in removing matrix components was observed when primary secondary amine (PSA) sorbent was introduced into the blending operation. The developed method was fully validated, and the limits of detection for BPA and BPB were 20 μg/kg and 30 μg/kg, respectively. Average recoveries and precisions were ranged from 83.03% to 94.64% and 1.76% to 5.45%, respectively. This is the first report on the analysis of bisphenol contaminants in bee pollen sample, and also on the combination of MSPD and HLLE. The present method might provide a new strategy for simple and fast sample preparation of solid and semi-solid samples.


2014 ◽  
Vol 69 (4) ◽  
Author(s):  
Norfahana Abd-Talib ◽  
Siti Hamidah Mohd-Setapar ◽  
Aidee Kamal Khamis

Over recent years, there has been an explosive growth of sample preparation techniques. Sample preparation is in most cases meant to be the isolation online or offline concentration of some components of interest or target analytes. Solid phase extraction (SPE) is a very popular technique nowadays in sample preparation. The principal is quite similar with liquid- liquid extraction (LLE) which involves partition of solutes between two phases. But, there are some differences between them and some benefits and limitations of difference types of SPE technique like presented in this paper.


Author(s):  
RIMADANI PRATIWI ◽  
RASPATI D. MULYANINGSIH ◽  
NYI M. SAPTARINI

Objective: This study was aimed to understand and determine the effectiveness of allopurinol extraction in herbal medicine from three extraction methods based on parameters of accuracy and precision. Methods: The study consisted of three methods including dissolving and filtering, liquid-liquid extraction, and solid-phase extraction with mixed-mode cation exchanger (SPE-MCX). The procedures were carried out using NaOH and HCl in dissolving and filtering method; methanol, HCl, and ethyl acetate in liquid-liquid extraction; and NH4OH elution solvent in SPE-MCX. Results: The results showed that extraction effectiveness based on accuracy level was the dissolving and filtering method>SPE-MCX>liquid-liquid extraction with % recovery+SD of 91.314+2.903%, 87.533+4.950%, and 54.549+3.517%, respectively. The precision level was the dissolution and filtering method>SPE-MCX>liquid-liquid extraction based on % relative standard deviations (RSD) of 3.18%, 5.226%, and 6.446%, respectively. Conclusion: It can be concluded that the allopurinol extraction method with the highest effectiveness based on accuracy and precision parameters in herbal medicine is the dissolving and filtering method.


2019 ◽  
Vol 6 (8) ◽  
pp. 190952 ◽  
Author(s):  
Nur Hidayah Sazali ◽  
Anas Alshishani ◽  
Bahruddin Saad ◽  
Ker Yin Chew ◽  
Moi Me Chong ◽  
...  

In this study, salting-out assisted liquid–liquid extraction (SALLE) as a simple and efficient extraction technique followed by high-performance liquid chromatography (HPLC) was employed for the determination of vitamin D3 in milk samples. The sample treatment is based on the use of water-miscible acetonitrile as the extractant and acetonitrile phase separation under high-salt conditions. Under the optimum conditions, acetonitrile and ammonium sulfate were used as the extraction solvent and salting-out agent, respectively. The vitamin D3 extract was separated using Hypersil ODS (250x i.d 4.6 mm, 5 µm) HPLC column that was coupled with diode array detector. Vitamin D2 was used as internal standard (IS) to offset any variations in chromatographic conditions. The vitamin D3 and the IS were eluted in 18 min. Good linearity ( r 2 > 0.99) was obtained within the range of 25–600 ng g −1 with the limit of detection of 15 ng g −1 and limit of quantification of 25 ng g −1 . The validated method was applied for the determination of vitamin D3 in milk samples. The recoveries for spiked samples were from 94.4 to 113.5%.


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