Automated sample preparation station for studying self-diffusion in porous solids with NMR spectroscopy

2006 ◽  
Vol 77 (3) ◽  
pp. 035114 ◽  
Author(s):  
Niklas Hedin ◽  
Gregory J. DeMartin ◽  
Sebastián C. Reyes
Keyword(s):  
Nmr Spectroscopy ◽  
Sample Preparation ◽  
Porous Solids ◽  
Self Diffusion ◽  
Automated Sample Preparation

Controlling Gas Selectivity in Molecular Porous Liquids by Tuning the Cage Window Size

2019 ◽  
Author(s):  
Benjamin Egleston ◽  
Konstantin V. Luzyanin ◽  
Michael C. Brand ◽  
Rob Clowes ◽  
Michael E. Briggs ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Chemical Synthesis ◽  
Field Gradient ◽  
Window Size ◽  
Standard Approach ◽  
Porous Solids ◽  
Pulsed Field Gradient Nmr ◽  
Pulsed Field ◽  
Cage Molecules ◽  
Gas Selectivity

Control of pore window size is the standard approach for tuning gas selectivity in porous solids. Here, we present the first example where this is translated into a molecular porous liquid formed from organic cage molecules. Reduction of the cage window size by chemical synthesis switches the selectivity from Xe-selective to CH<sub>4</sub>-selective, which is understood using <sup>129</sup>Xe, <sup>1</sup>H, and pulsed-field gradient NMR spectroscopy.

Controlling Gas Selectivity in Molecular Porous Liquids by Tuning the Cage Window Size

2019 ◽  
Author(s):  
Benjamin Egleston ◽  
Konstantin V. Luzyanin ◽  
Michael C. Brand ◽  
Rob Clowes ◽  
Michael E. Briggs ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Chemical Synthesis ◽  
Field Gradient ◽  
Window Size ◽  
Standard Approach ◽  
Porous Solids ◽  
Pulsed Field Gradient Nmr ◽  
Pulsed Field ◽  
Cage Molecules ◽  
Gas Selectivity

Control of pore window size is the standard approach for tuning gas selectivity in porous solids. Here, we present the first example where this is translated into a molecular porous liquid formed from organic cage molecules. Reduction of the cage window size by chemical synthesis switches the selectivity from Xe-selective to CH<sub>4</sub>-selective, which is understood using <sup>129</sup>Xe, <sup>1</sup>H, and pulsed-field gradient NMR spectroscopy.

scholarly journals The Application of NMR Spectroscopy and Chemometrics in Authentication of Spices

Molecules ◽  
2021 ◽  
Vol 26 (2) ◽  
pp. 382
Author(s):  
Barbara Pacholczyk-Sienicka ◽  
Grzegorz Ciepielowski ◽  
Łukasz Albrecht
Keyword(s):  
Quality Assurance ◽  
Nmr Spectroscopy ◽  
Sample Preparation ◽  
Bioactive Compounds ◽  
Analytical Methods ◽  
Structural Information ◽  
Chemometric Analysis ◽  
Spectroscopic Methods ◽  
Regular Consumption ◽  
No Sample Preparation

Spices and herbs are among the most commonly adulterated food types. This is because spices are widely used to process food. Spices not only enhance the flavor and taste of food, but they are also sources of numerous bioactive compounds that are significantly beneficial for health. The healing effects of spices are connected with their antimicrobial, anti-inflammatory and carminative properties. However, regular consumption of adulterated spices may cause fatal damage to our system because adulterants in most cases are unhealthy. For that reason, the appropriate analytical methods are necessary for quality assurance and to ensure the authenticity of spices. Spectroscopic methods are gaining interest as they are fast, require little or no sample preparation, and provide rich structural information. This review provides an overview of the application of NMR spectroscopy combined with chemometric analysis to determine the quality and adulteration of spices.

Optimization of Automated Sample Preparation for Vitamin D Determination on a Biomek i7 Workstation

2021 ◽  
pp. 247263032110302
Author(s):  
Anna Bach ◽  
Heidi Fleischer ◽  
Bhagya Wijayawardena ◽  
Kerstin Thurow
Keyword(s):  
Vitamin D ◽  
Sample Preparation ◽  
Reference Method ◽  
Positive Pressure ◽  
Additional Risk Factor ◽  
Serum Samples ◽  
Recovery Rates ◽  
Preparation Methods ◽  
Sample Throughput ◽  
Automated Sample Preparation

Vitamin D belongs to the fat-soluble vitamins and is an integral part of bone metabolism. In the human body, a decreased vitamin D level can be an additional risk factor for diseases like cancer, diabetes, and mental diseases. As a result, an enormous increase in the demand for vitamin D testing has been observed in recent years, increasing the demand for powerful methods for vitamin D determination at the same time. Automation is the key factor in increasing sample throughput. This study compares three fully automated sample preparation methods for the determination of 25(OH)D2 and 25(OH)D3 in plasma and serum samples. Starting from a semiautomated reference method, the method is tested manually and subsequently fully automated on the Biomek i7 Workstation by integrating a centrifuge and a positive pressure extractor into the workstation. Alternatively, the centrifugation for the separation of protein aggregates and supernatant is replaced by a filter plate. Finally, the sample throughput is further increased by using phospholipid removal cartridges. The results show that phospholipid removal significantly increases the recovery rates in liquid chromatography–mass spectrometry. With the phospholipid removal cartridges, recovery rates of 97.36% for 25(OH)D2 and 102.5% for 25(OH)D3 were achieved, whereas with the automated classic automated preparation method, the recovery rates were 83.31% for 25(OH)D2 and 86.54% for 25(OH)D3. In addition to the technical evaluation, the different methods were also examined with regard to their economic efficiency. Finally, the qualitative and quantitative performance of the developed methods is benchmarked with a selected semiautomatic reference method.

scholarly journals Automated Sample Preparation and Data Collection Workflow for High-Throughput In Vitro Metabolomics

Metabolites ◽  
2022 ◽  
Vol 12 (1) ◽  
pp. 52
Author(s):  
Julia M. Malinowska ◽  
Taina Palosaari ◽  
Jukka Sund ◽  
Donatella Carpi ◽  
Gavin R. Lloyd ◽  
...  
Keyword(s):  
Sample Preparation ◽  
High Throughput ◽  
High Throughput Screening ◽  
In Vitro Screening ◽  
Chemical Safety ◽  
Experimental Conditions ◽  
Well Location ◽  
Relative Standard ◽  
Automated Sample Preparation

Regulatory bodies have started to recognise the value of in vitro screening and metabolomics as two types of new approach methodologies (NAMs) for chemical risk assessments, yet few high-throughput in vitro toxicometabolomics studies have been reported. A significant challenge is to implement automated sample preparation of the low biomass samples typically used for in vitro screening. Building on previous work, we have developed, characterised and demonstrated an automated sample preparation and analysis workflow for in vitro metabolomics of HepaRG cells in 96-well microplates using a Biomek i7 Hybrid Workstation (Beckman Coulter) and Orbitrap Elite (Thermo Scientific) high-resolution nanoelectrospray direct infusion mass spectrometry (nESI-DIMS), across polar metabolites and lipids. The experimental conditions evaluated included the day of metabolite extraction, order of extraction of samples in 96-well microplates, position of the 96-well microplate on the instrument’s deck and well location within a microplate. By using the median relative standard deviation (mRSD (%)) of spectral features, we have demonstrated good repeatability of the workflow (final mRSD < 30%) with a low percentage of features outside the threshold applied for statistical analysis. To improve the quality of the automated workflow further, small method modifications were made and then applied to a large cohort study (4860 sample infusions across three nESI-DIMS assays), which confirmed very high repeatability of the whole workflow from cell culturing to metabolite measurements, whilst providing a significant improvement in sample throughput. It is envisioned that the automated in vitro metabolomics workflow will help to advance the application of metabolomics (as a part of NAMs) in chemical safety, primarily as an approach for high throughput screening and prioritisation.

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