scholarly journals Qualitative and Quantitative Comparison of Liquid–Liquid Phase Extraction Using Ethyl Acetate and Liquid–Solid Phase Extraction Using Poly-Benzyl-Resin for Natural Products

2021 ◽  
Vol 11 (21) ◽  
pp. 10241
Author(s):  
Yannik K. Schneider ◽  
Solveig M. Jørgensen ◽  
Jeanette Hammer Andersen ◽  
Espen H. Hansen

A key step in the process of isolating microbial natural products is the preparation of an extract from a culture. This step determines which molecules will be available for detection in the subsequent chemical and biological analysis of a biodiscovery pipeline. In the present study we wanted to document potential differences in performance between liquid–liquid extraction using ethyl acetate and liquid–solid extraction using a poly-benzyl-resin. For the comparison of the two extraction protocols, we spiked a culture of Flavobacterium sp. with a diverse selection of natural products of microbial and plant origin to investigate whether the methods were comparable with respect to selectivity. We also investigated the efficiency of the two extraction methods quantitatively, using water spiked with a selection of natural products, and studied the quantitative effect of different pH levels of the aqueous solutions on the extraction yields of the two methods. The same compounds were extracted by the two methods, but the solid-phase extract contained more media components compared with the liquid-phase extract. Quantitatively, the two extraction methods varied in their recovery rates. We conclude that practical aspects could be more important when selecting one of the extraction protocols, as their efficiencies in extracting specific compounds were quite similar.

Weed Science ◽  
1996 ◽  
Vol 44 (3) ◽  
pp. 689-693 ◽  
Author(s):  
Melissa B. Riley ◽  
Renee J. Keese

Solid phase extraction (SPE) procedures were used to determine the recoveries of herbicides typically used in containerized ornamental plant production from water samples. Recoveries from C18cartridges and disks were compared for each of 12 herbicides with variations in elution solvent and volume of elution solvent tested. Recoveries for nine of the herbicides from the cartridges and disks using acetone as an elution solvent were not affected by SPE matrix. Fluazifop recovery was greater with the disks, while napropamide and oxadiazon recoveries were greater with cartridges. Both cartridges and disks yielded low recoveries (23 to 47%) of benefin and prodiamine. Changing the elution solvent from acetone to acetonitrile resulted in 10% improvement for the recovery of benefin and a three- to four-fold increase in recovery of prodiamine. Acetonitrile decreased recoveries of napropamide, oryzalin, oxadiazon, oxyfluorfen, and pendimethalin from cartridges. For the disks, oxyfluorfen, prodiamine, and trifluralin had increased recovery, while fluazifop, oxadiazon, and simazine had decreased recovery with acetonitrile as the elution solvent. Increasing the amount of acetone eluting solvent increased the recovery of prodiamine and oxyfluorfen while decreasing the recovery of fluazifop, pendimethalin, simazine, and trifluralin. Binding capacities of oryzalin on cartridges and disks averaged 13.2 and 7.8 mg, respectively. The advantage of the disk lies in the greater volume of water that can be processed, while the higher cost and greater variability are disadvantages. Cartridge extraction yielded good recoveries with lower standard deviations, and used less organic solvent. Selection of an SPE extraction method depends upon the herbicides under evaluation, expected levels, and the water volume being processed. Both SPE techniques offer advantages over traditional liquid-liquid extraction methods such as reduced requirements for organic solvent and sample preparation.


2016 ◽  
Vol 9 (1) ◽  
pp. 30
Author(s):  
Wei Zhang ◽  
Jun Wang ◽  
Zhiyuan Mi ◽  
Jiangtao Su ◽  
Xiangyu You ◽  
...  

Although misuse and abuse of Cannabis is well known, the health benefits have been proved by various biomedical studies. Tetrahydrocannabinol (THC) is the major active substance in leaves of Cannabis, which is the common target for drug testing. In field drug testing, oral fluid (OF) has its unique advantages over other specimens such as blood, urine, and hair. Thus the study of THC in OF is gaining popularity in Cannabis research. In this review, extraction methods are introduced in three categories, which are Liquid-Liquid Extraction (LLE), Solid Phase Extraction (SPE), and Supercritical Fluid Extraction (SFE). Examples of application with each method will be covered. Advantages and disadvantages of these methods will be compared. In addition, methods in analysis following extraction will be briefly discussed.


Separations ◽  
2019 ◽  
Vol 6 (4) ◽  
pp. 53 ◽  
Author(s):  
Katarzyna Madej ◽  
Wojciech Piekoszewski

The current clinical and forensic toxicological analysis of body fluids requires a modern approach to sample preparation characterized by high selectivity and enrichment capability, suitability for micro-samples, simplicity and speed, and the possibility of automation and miniaturization, as well as the use of small amounts of reagents, especially toxic solvents. Most of the abovementioned features may be realized using so-called microextraction techniques which cover liquid-phase techniques (e.g., single-drop microextraction, SDME; dispersive liquid–liquid microextraction, DLLME; hollow-fiber liquid-phase microextraction, HF-LPME) and solid-phase extraction techniques (solid-phase microextraction, SPME; microextraction in packed syringes, MEPS; disposable pipette tip extraction, DPX; stir bar sorption extraction, SBSE). Some other extraction methodologies like dispersive solid-phase extraction (d-SPE) or magnetic solid-phase extraction (MSPE) can also be easily miniaturized. This review briefly describes and characterizes the abovementioned extraction methods, and then presents their current applications to the preparation of body fluids analyzed for bioactive compounds in combination with appropriate analytical methods, mainly chromatographic and related techniques. The perspectives of the analytical area we are interested in are also indicated.


2016 ◽  
Vol 52 (2) ◽  
pp. 107-114
Author(s):  
Barbara Potocka-Banaś ◽  
Teresa Dembińska ◽  
Krzysztof Borowiak

The aim of the study was to compare efficiency of various extraction methods of benzodiazepine derivatives: diazepam, estazolam, flunitrazepam and nitrazepam. The study compared the recovery of benzodiazepines isolated from biological material (blood and human blood serum) using liquid-liquid extraction and solid-phase extraction. The efficiency of each extraction was evaluated using high-performance liquid chromatography with diode array detector. In addition, benzodiazepines immunoassay reactivity was estimated. The following methods of extraction were used: liquid-liquid extraction (a classical liquid-liquid extraction and microextraction), solid- -phase extraction (Baker’s columns and United Chemical Technologies’ (UTC columns). The reactivity was evaluated using V-Twin System with EMIT technology by Siemens. The results showed that the lowest recovery (nitrazepam – 16%, diazepam – 23%, flunitrazepam – 28%, estazolam – 37%) was obtained using liquid-liquid microextraction of whole blood and the highest recovery was obtained in solid-phase extraction of whole blood using United Chemical Technologies’ columns (nitrazepam – 86%, diazepam – 89%, estazolam – 91%, flunitrazepam – 94%). The lowest recovery in classical liquid-liquid extraction was obtained for diazepam isolated from whole blood (36%), and the highest – for flunitrazepam isolated from serum (74%). Solid-phase extraction with Baker’s columns was successful only in case of drugs isolation from serum and the recovery range from 57% to 89% for flunitrazepam. The results indicated higher efficiency of solid-phase extraction, especially with use of columns specific for the extraction of benzodiazepines. The immunoassay analysis showed a decreased reactivity of the tested benzodiazepine derivatives on the reagent used for the EMIT assay. Comparative analysis of the recovery efficiency of selected benzodiazepine derivatives led to the conclusion that use of solid-phase extraction should be considered more often in routine toxicological analysis. The knowledge of benzodiazepine derivatives cross-reactivity in immunoassay method is essential for correct interpretation of obtained results.


2017 ◽  
Vol 2017 ◽  
pp. 1-7 ◽  
Author(s):  
Hale Seçilmiş Canbay

Steam distillation is used to isolate scent of rose flowers. Rose aromatic water is commonly used in European cuisine and aromatherapy besides its use in cosmetic industry for its lovely scent. In this study, three different sampling techniques, liquid-liquid extraction (LLE), headspace technique (HS), and solid phase extraction (SPE), were compared for the analysis of volatile water-soluble compounds in commercial rose aromatic water. Some volatile water-soluble compounds of rose aromatic water were also analyzed by gas chromatography mass spectrometry (GCMS). In any case, it was concluded that one of the solid phase extraction methods led to higher recoveries for 2-phenylethyl alcohol (PEA) in the rose aromatic water than the liquid-liquid extraction and headspace technique. Liquid-liquid extraction method provided higher recovery ratios for citronellol, nerol, and geraniol than others. Ideal linear correlation coefficient values were observed by GCMS for quantitative analysis of volatile compounds (r2≥0.999). Optimized methods showed acceptable repeatability (RSDs < 5%) and excellent recovery (>95%). For compounds such as α-pinene, linalool, β-caryophyllene, α-humulene, methyl eugenol, and eugenol, the best recovery values were obtained with LLE and SPE.


2017 ◽  
Vol 8 (2) ◽  
pp. 106
Author(s):  
Rosy Hutami ◽  
N Idzni ◽  
R Ranasasmita ◽  
Mira Suprayatmi

Dalam teknik deteksi molekuler seperti Loop-Amplification Mediated Polymorphism (LAMP) dan Polymerase Chain Reaction (PCR), pembuatan hulu asam deoksiribonukleat (DNA) sangat penting. Ekstraksi fase cair dan ekstraksi fasa padat merupakan beberapa metode ekstraksi DNA yang tersedia. Tujuan dari penelitian ini adalah untuk mengkarakterisasi metode dan produk ekstraksi DNA berdasarkan kemurnian DNA, visualisasi DNA, konsentrasi DNA, dan waktu pemrosesan metode ekstraksi DNA. Metode ekstraksi yang dievaluasi meliputi metode fenol-kloroform (Metode A) sebagai ekstraksi fasa cair dan metode Ekstraksi Surefood kit (Metode B) sebagai ekstraksi fasa padat. Hasil penelitian menunjukkan bahwa Metode A dapat dilakukan pada sampel dengan konsentrasi DNA sangat rendah berkisar antara 7,00 sampai 9,45 ng / μl dengan kemurnian yang baik (1,80-2,10). Meski tidak menunjukkan DNA isolat band pada gel agarosa 1% dan membutuhkan waktu pemrosesan ± 30 jam. Metode B memiliki performa yang baik dalam mengekstraksi sampel dengan DNA dengan konsentrasi tinggi (49,67 sampai 357,28 ng / μl) dengan kemurnian yang baik (1,93 sampai 2,07). Metode ini menunjukkan band untuk setiap sampel DNA pada gel agarose 1% dan membutuhkan waktu ±1 jam. Kedua metode tersebut dapat digunakan untuk preparasi sampel dalam analisis molekuler termasuk tujuan otentikasi halal.KATA KUNCI: fenol, kloroform, Surefood kit, LAMP  DNA EXTRACTION METHOD FOR MOLECULAR DETECTIONABSTRACTIn molecular detection technique such as Loop-Amplification Mediated Polymorphism (LAMP) and Polymerase Chain Reaction (PCR), right upstream preparation of deoxyribonucleic acid (DNA) is very important. Liquid phase extraction and solid phase extraction are some of DNA extraction methods those are available. The purpose of this research was to characterizedthe method and product of DNA extraction based on DNA purity, DNA visualization, DNA concentration, and processing time of DNA extraction methods. Extraction methods evaluated included phenol-chloroform method (Method A)as liquid phase extraction and Surefood Extraction kit method (Method B) as solid phase extraction. Result showed that Method A could be performed on samples with very low DNA concentrations ranging from 7.00 to 9.45 ng/µl with a good purity (1.80 to 2.10). Although,  it showed no DNA isolates bands on gel agarose 1% and need ± 30 hours processing time. Method B had a good performa in extracting sample with high concentration DNA (49.67 to 357.28 ng/µl) with a good purity (1.93 to 2.07). This method showed bands for each DNA samples on gel agarose 1% and need about ± 1 hour processing time. Both methods can be used for sample preparation in molecular analysis including halal authentication purposes.  


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