scholarly journals Sample preparation for the analysis of key metabolites from cannabinoids biosynthesis in phytoplankton using GC-MS

2021 ◽  
Author(s):  
Liyun Ye ◽  
Suzanne Budge
Keyword(s):  
Sample Preparation ◽  
Solid Phase ◽  
Degradation Products ◽  
Rapid Development ◽  
Isochrysis Galbana ◽  
Graphitized Carbon Black ◽  
Gas Chromatography Mass Spectrometry ◽  
Ms Analysis ◽  
Strong Anion Exchange ◽  
Transformation Methods

Cannabinoids biosynthesis in phytoplankton has attracted much attention due to the rapid development of genetic tools and the optimization of genetic transformation methods in microalgae. To monitor the biosynthesis process, proper sample preparation and practical instrumental methods are needed to measure the various precursors, intermediates, cannabinoids, and their degradation products. The objective of this study was to develop a sample preparation procedure for the quantification of olivetolic acid (OA), cannabigerolic acid (CBGA), cannabidiolic acid (CBDA), tetrahydrocannabinolic acid (THCA), olivetol (OL), cannabidiol (CBD), and tetrahydrocannabinol (THC) using single-quadrupole gas chromatography-mass spectrometry (GC-MS). Isochrysis galbana was used as the model matrix. After methanol extraction, samples were purified using solid phase extraction (SPE), silylated with N-methyl-N-(trimethylsilyl)trifluoroacetamide, and analyzed using GC-MS in electron ionization mode. A strong anion-exchange SPE efficiently recovered OA, CBGA, CBDA, and THCA. A graphitized carbon black SPE was necessary to purify OL, CBD, and THC. Both columns removed amino acids, sugars, polyols, and pigments from the algae extract and prepared samples that are suitable for silylation and GC-MS analysis. The total protocol, including solvent extraction, SPE, silylation, and GC-MS analysis, was validated in accordance with the ICH guidelines. Performance characteristics of our method are superior to existing protocols with similar complexity in the literature.

scholarly journals An Effective and Efficient Sample Preparation Method for 2-Methyl-Isoborneol and Geosmin in Fish and Their Analysis by Gas Chromatography-Mass Spectrometry

2021 ◽  
Vol 2021 ◽  
pp. 1-8
Author(s):  
Liang-liang Tian ◽  
Feng Han ◽  
Essy Kouadio Fodjo ◽  
Wenlei Zhai ◽  
Xuan-Yun Huang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Sample Preparation ◽  
Large Scale ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Ms Analysis ◽  
Fish Samples

The intensive aquaculture strategy and recirculating aquaculture system often lead to the production of off-flavor compounds such as 2-methyl-isoborneol (2-MIB) and Geosmin (GSM). The regular purge and trap extraction followed by analysis with gas chromatography-mass spectrometry (GC-MS) usually involve a complicated assembly of facilities, more working space, long sample preparation time, and headspace solid-phase microextraction (SPME). In this work, a method with easier sample preparation, fewer and simplified facilities, and without SPME on GC-MS analysis is developed for the determination of 2-MIB and GSM in fish samples. Unlike previous methods, solvent extract from samples, QuEChERS-based cleanup, and solid-phase extraction for concentration are applied. The LOD (S/N > 3) and LOQ (S/N > 10) of this method were validated at 0.6 μg/kg and 1.0 μg/kg for both 2-MIB and GSM, which are under the sensory limit (1 μg/kg). Application of this method for incurred fish samples demonstrated acceptable analytical performance. This method is suitable for large-scale determination of 2-MIB and GSM in fish samples, owing to the use of simple facility and easy-to-operate procedure, rapid sample preparation, and shorter time for GC-MS analysis without SPME.

scholarly journals Optimisation of Urine Sample Preparation for Headspace-Solid Phase Microextraction Gas Chromatography-Mass Spectrometry: Altering Sample pH, Sulphuric Acid Concentration and Phase Ratio

Metabolites ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 482
Author(s):  
Prashant Aggarwal ◽  
James Baker ◽  
Mark T. Boyd ◽  
Séamus Coyle ◽  
Chris Probert ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Sample Preparation ◽  
Urine Sample ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Headspace Solid Phase Microextraction ◽  
Chromatography Mass Spectrometry ◽  
Ms Analysis

Headspace-solid phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS) can be used to measure volatile organic compounds (VOCs) in human urine. However, there is no widely adopted standardised protocol for the preparation of urine samples for analysis resulting in an inability to compare studies reliably between laboratories. This paper investigated the effect of altering urine sample pH, volume, and vial size for optimising detection of VOCs when using HS-SPME-GC-MS. This is the first, direct comparison of H2SO4, HCl, and NaOH as treatment techniques prior to HS-SPME-GC-MS analysis. Altering urine sample pH indicates that H2SO4 is more effective at optimising detection of VOCs than HCl or NaOH. H2SO4 resulted in a significantly larger mean number of VOCs being identified per sample (on average, 33.5 VOCs to 24.3 in HCl or 12.2 in NaOH treated urine) and more unique VOCs, produced a more diverse range of classes of VOCs, and led to less HS-SPME-GC-MS degradation. We propose that adding 0.2 mL of 2.5 M H2SO4 to 1 mL of urine within a 10 mL headspace vial is the optimal sample preparation prior to HS-SPME-GC-MS analysis. We hope the use of our optimised method for urinary HS-SPME-GC-MS analysis will enhance our understanding of human disease and bolster metabolic biomarker identification.

scholarly journals Effect of Blender and Blending Time on Color and Aroma Characteristics of Juice and Its Freeze-Dried Powder of Pandanus amaryllifolius Roxb. Leaves (Pandan)

2016 ◽  
Vol 12 (1) ◽  
pp. 75-81 ◽  
Author(s):  
Kandhasamy Sowndhararajan ◽  
Nyuk Ling Chin ◽  
Yus Aniza Yusof ◽  
Lee Ling Lai ◽  
Wan Aida Wan Mustapha
Keyword(s):  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Particle Size Reduction ◽  
Ms Analysis ◽  
Freeze Dried ◽  
Aroma Characteristics ◽  
Mechanical Extraction ◽  
Aroma Components ◽  
Color Pigment ◽  
Pandanus Amaryllifolius

Abstract The color and aroma properties of Pandanus amaryllifolius Roxb. leaves (pandan) were studied by mechanical extraction using normal and turbo blade blenders under different blending times (60–180 s). The extracted juice was freeze-dried into powders and its aroma components were measured in a solid-phase microextraction using gas chromatography/mass spectrometry (SPME-GC/MS) analysis. The turbo blade blender provided maximum color pigment of greenness and yellowness at blending time of 90 s as compared to the normal blender that required 180 s. In GC-MS analysis, the major component, 2-acetyl-1-pyrroline, was found to be one time higher in the freeze-dried pandan juice samples obtained from turbo blade blender than normal blender. Other components including the cis-3-hexanal, 2-methylene-4-pentenenitrile and 1,2,4-trimethylbenzene were also detected in the samples. In conclusion, the turbo blade blender is more effective than normal laboratory blender in terms of color extraction, particle size reduction and the aroma retention.

scholarly journals Modern Methods of Sample Preparation for the Analysis of Oxylipins in Biological Samples

Molecules ◽  
2019 ◽  
Vol 24 (8) ◽  
pp. 1639 ◽  
Author(s):  
Liakh ◽  
Pakiet ◽  
Sledzinski ◽  
Mika
Keyword(s):  
Mass Spectrometry ◽  
Sample Preparation ◽  
Biological Samples ◽  
Solid Phase ◽  
Biological Tissues ◽  
Gas Chromatography Mass Spectrometry ◽  
Liquid Liquid Extraction ◽  
Wide Range ◽  
Popular Subject ◽  
Technological Platforms

Oxylipins are potent lipid mediators derived from polyunsaturated fatty acids, which play important roles in various biological processes. Being important regulators and/or markers of a wide range of normal and pathological processes, oxylipins are becoming a popular subject of research; however, the low stability and often very low concentration of oxylipins in samples are a significant challenge for authors and continuous improvement is required in both the extraction and analysis techniques. In recent years, the study of oxylipins has been directly related to the development of new technological platforms based on mass spectrometry (LC–MS/MS and gas chromatography–mass spectrometry (GC–MS)/MS), as well as the improvement in methods for the extraction of oxylipins from biological samples. In this review, we systematize and compare information on sample preparation procedures, including solid-phase extraction, liquid–liquid extraction from different biological tissues.

scholarly journals Comparison of an Offline SPE–GC–MS and Online HS–SPME–GC–MS Method for the Analysis of Volatile Terpenoids in Wine

Molecules ◽  
2020 ◽  
Vol 25 (3) ◽  
pp. 657 ◽  
Author(s):  
Cody Williams ◽  
Astrid Buica
Keyword(s):  
Sample Preparation ◽  
Solid Phase ◽  
White Wine ◽  
Gas Chromatography Mass Spectrometry ◽  
Wine Quality ◽  
White Wines ◽  
Preparation Methods ◽  
Odor Thresholds ◽  
Spe Method ◽  
Sample Preparation Methods

The aroma profile is an important marker for wine quality. Various classes of compounds are responsible for the aroma of wine, and one such class is terpenoids. In the context of this work, a validated gas chromatography–mass spectrometry (GC–MS) method for the quantitation of terpenoids in red and white wine using headspace solid-phase microextraction (HS–SPME) and solid-phase extraction (SPE) was established. Calibrations were performed in the respective base wine using both sample preparation methods. The linearity, precision and accuracy evaluated for the respective matrices were excellent for both sample preparations. However, the HS–SPME approach was more sensitive and more accurate. For both sample preparations, the quantification limits were lower than the odor thresholds in wine. The terpenoid concentrations (µg/L) were evaluated for 13 white wines using both sample preparation methods. Importantly, the online HS–SPME approach was more sensitive than the offline SPE method. The major terpenoids identified in the white wines evaluated were linalool (0.2–63 µg/L), geraniol (nd–66 µg/L) and α-terpineol (nd–85 µg/L).

Chemometric Study and Optimization of Headspace Solid-Phase Microextraction Parameters for the Determination of Multiclass Pesticide Residues in Processed Cocoa from Nigeria Using Gas Chromatography/Mass Spectrometry

2014 ◽  
Vol 97 (4) ◽  
pp. 1007-1011 ◽  
Author(s):  
Lukman Bola Abdulra'uf ◽  
Guan Huat Tan
Keyword(s):  
Sample Preparation ◽  
Pesticide Residues ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Internal Standard ◽  
Calibration Method ◽  
Gas Chromatography Mass Spectrometry ◽  
Design Matrix ◽  
Analytical Methodology ◽  
Cocoa Powder

Abstract Solid-phase microextraction (SPME) is a solventless sample preparation method that combines sample preparation, isolation, concentration, and enrichment into one step. A simple and effective method coupling headspace-SPME to GC/MS was developed for the analysis of chlorpyrifos, fenitrothion, endosulfan I, and endosulfan II pesticide residues in cocoa powder. In this study, multivariate strategy was used to determine the significance of the factors affecting the SPME of the pesticides using a Plackett-Burman design, and the significant factors were optimized using central composite design. The analytes were extracted with 100 μm polydimethylsiloxane fibers according to the factorial design matrix and desorbed into a GC/MS instrument. The developed method was applied for the analysis of a cocoa powder sample, and it exhibited good figures of merit for the analytical methodology. Using the optimized conditions, the linearity ranged from 2.5 to 500 μg/kg (R2 > 0.99) using an internal standard calibration method, and the average recoveries were between 75 and 95%, with RSD values between 3.8 and 9.7%.

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