scholarly journals Optimization of Residual Hexane in Edible Oils Analysis Using Static Headspace Gas Chromatography

2021 ◽  
Vol 2021 ◽  
pp. 1-6
Author(s):  
Azrul Hisyam Samsuri ◽  
May Yen Ang ◽  
Shean Yeaw Ng
Keyword(s):  
Gas Chromatography ◽  
Edible Oils ◽  
Fats And Oils ◽  
The European Union ◽  
Limit Of Quantification ◽  
Efficient Manner ◽  
Residual Hexane ◽  
Automated Method ◽  
Static Headspace Gas Chromatography ◽  
Significant Difference

This study aims to determine the residual hexane in four edible oils in Malaysia using a simple, rapid, and automated method in order to improve the efficiency and productivity of the analysis. Gas chromatography (GC/FID) equipped with a headspace autosampler (HS-20) was used to perform the analysis. Incubation time for each injection was successfully optimized from one hour to 30 minutes (50% reduction) compared to the official AOCS method Ca 3b-87. Out of the four tested edible oils, only the hexane residues detected in sunflower oil exceeded the maximum residue limit (MRL) set by the European Union regulation. Significant difference of the results obtained between large calibration range (0–938 mg kg−1) and small calibration range (0–68 mg kg−1) suggests that there is a need to use a lower standard calibration concentration to avoid misinterpretation of analysis results. Method validation applies to the technical hexane; 2-methylpentane, 3-methylpentane, cyclohexane, and methylcyclopentane, the signal-to-noise (S/N), as well as the limit of quantification (LoQ) values was found to be 218.20, 221.45, 746.37, 97.37 and 0.85, 0.84, 0.25, 1.93 mg kg−1, respectively. Good linearity, repeatability, and low carryover of this method have provided an alternative way to analyze the content of the residual hexane in edible oils in a more efficient manner. Current study might provide a fundamental reference for the improvement of the AOCS official Ca 3b-87 method for determination of hexane residues in fats and oils analysis in the future.

Feasibility and Evaluation of Automated Methods for Radiolabeling of Radiopharmaceutical Kits with Gallium-68

2019 ◽  
Vol 12 (3) ◽  
pp. 229-237 ◽  
Author(s):  
Alban Revy ◽  
François Hallouard ◽  
Sandrine Joyeux-Klamber ◽  
Andrea Skanjeti ◽  
Catherine Rioufol ◽  
...  
Keyword(s):  
The European Union ◽  
Preparation Time ◽  
Limit Of Quantification ◽  
Manual Method ◽  
Personnel Costs ◽  
Automated Method ◽  
Gallium 68 ◽  
The Right ◽  
First Time ◽  
Automated Methods

Objective: Recent gallium-68 labeled peptides are of increasing interest in PET imaging in nuclear medicine. Somakit TOC® is a radiopharmaceutical kit registered in the European Union for the preparation of [68Ga]Ga-DOTA-TOC used for the diagnosis of neuroendocrine tumors. Development of a labeling process using a synthesizer is particularly interesting for the quality and reproducibility of the final product although only manual processes are described in the Summary of Product (SmPC) of the registered product. The aim of the present study was therefore to evaluate the feasibility and value of using an automated synthesizer for the preparation of [68Ga]Ga-DOTA-TOC according to the SmPC of the Somakit TOC®. Methods: Three methods of preparation were compared; each followed the SmPC of the Somakit TOC®. Over time, overheads, and overexposure were evaluated for each method. Results: Mean±SD preparation time was 26.2±0.3 minutes for the manual method, 28±0.5 minutes for the semi-automated, and 40.3±0.2 minutes for the automated method. Overcost of the semi-automated method is 0.25€ per preparation for consumables and from 0.58€ to 0.92€ for personnel costs according to the operator (respectively, technician or pharmacist). For the automated method, overcost is 70€ for consumables and from 4.06€ to 6.44€ for personnel. For the manual method, extremity exposure was 0.425mSv for the right finger, and 0.350mSv for the left finger; for both the semi-automated and automated method extremity exposure were below the limit of quantification. Conclusion: The present study reports for the first time both the feasibility of using a [68Ga]- radiopharmaceutical kit with a synthesizer and the limits for the development of a fully automated process.

scholarly journals Microwave-Assisted Saponification Method Followed by Solid-Phase Extraction for the Characterization of Sterols and Dialkyl Ketones in Fats

Foods ◽  
2021 ◽  
Vol 10 (2) ◽  
pp. 445
Author(s):  
Steven Mascrez ◽  
Sabine Danthine ◽  
Giorgia Purcaro
Keyword(s):  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Reference Method ◽  
Fats And Oils ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Limit Of Quantification ◽  
Microwave Assisted

Unlike other fields, the methods routinely applied for fats and oils are still tied to traditional, time- and solvent-consuming procedures, such as saponification, column chromatography and thin-layer chromatography. In this paper, microwave-assisted saponification followed by a lab-made solid-phase extraction was optimized for the characterization of either dialkyl ketones (DAK) or sterols or both simultaneously. The instrumental determination was performed by gas chromatography- flame ionization detector (GC-FID) for quantification and gas chromatography-mass spectrometry (GC-MS) for confirmation purposes. The proposed method showed good recoveries (>80%) and limit of quantification (0.04–0.07 μg/g for the 4 DAK and of 0.07 μg/g for α-cholestanol). Repeatabilities (n = 3) were below 15% for DAKs and generally lower than 6% for sterols. Accuracy on the entire sterol profile was confirmed in comparison to the International Olive Council reference method. The method was finally applied to real-world samples before and after chemical interesterification.

scholarly journals Microbes a Tool for the Remediation of Organotin Pollution Determined by Static Headspace Gas Chromatography-Mass Spectrometry

2018 ◽  
Author(s):  
Christopher Finnegan ◽  
David Ryan ◽  
Ann-Marie Enright ◽  
Guiomar Garcia-Cabellos
Keyword(s):  
Gas Chromatography ◽  
Limit Of Detection ◽  
Gas Chromatography Mass Spectrometry ◽  
Headspace Gas Chromatography ◽  
Static Headspace ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Microbial Inoculant ◽  
Static Headspace Gas Chromatography ◽  
Headspace Gas

Tributyltin (TBT) is one of the most toxic anthropogenic compounds introduced into the marine environment. Despite its global ban in 2008, TBT is still a problem of great concern due to its high affinity for particulate matter, providing a direct and potentially persistent route of entry into benthic sediments. Bioremediation strategies may constitute an alternative approach to conventional physicochemical methods, benefiting from the microorganism’s potential to metabolize anthropogenic compounds. In this work, a simple, precise and accurate static headspace gas chromatography method was developed to investigate the ability of TBT degrading microbes in sedimentary microcosms over a period of 120 days. The proposed method was validated for linearity, repeatability, accuracy, specificity, limit of detection and limit of quantification. The method was subsequently successfully applied for the detection and quantification of TBT and degrading compounds in sediment samples on day 0, 30, 60, 90 and 120 of the experiment employing the principles of green chemistry. On day 120 the concentration of TBT remaining in the microcosms ranged between 91.91 ng/g wet wt for the least effective microbial inoculant to 52.73 ng/g wet wt for the most effective microbial inoculant from a stating concentration of 100 ng/g wet wt.

scholarly journals DETERMINATION OF RESIDUAL DIMETHYL SULFATE IN METHOXSALEN DRUG SUBSTANCE BY PRE-COLUMN DERIVATIZATION WITH STATIC HEADSPACE GAS CHROMATOGRAPHY

2018 ◽  
Vol 10 (8) ◽  
pp. 84
Author(s):  
Ajit Anerao ◽  
Bhushan Patil ◽  
Nitin Pradhan
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Dimethyl Sulfate ◽  
Drug Substance ◽  
Headspace Gas Chromatography ◽  
Limit Of Quantification ◽  
Static Headspace Gas Chromatography ◽  
Headspace Gas

Objective: Dimethyl sulfate has been highlighted as potential genotoxic and carcinogenic impurity. A sensitive Headspace gas chromatography (HS-GC) method with pre-column derivatization was developed and validated for the determination of dimethyl sulfate impurity in methoxsalen active pharmaceutical ingredient.Methods: HS-GC method on the column Agilent DB-5, 30m X 0.53 mm, film thickness 1.5 µm, with flame ionization detector (FID) was used. Derivatization reagent concentration, time of reaction and pH of the solution were optimized during method development. This analytical method was evaluated by performing method validation as per ICH guideline.Results: The proposed method was specific, linear, accurate, rugged and precise. The calibration curves showed good linearity over the concentration range of 0.5 μg/ml to 3.0 μg/ml and the correlation coefficient was 0.999. Method had very low limit of detection (LOD) and limit of quantification (LOQ) 2.0 μg/g and 5.0 μg/g respectively. Accuracy was observed within 98.1%–104.5%.Conclusion: The developed method was demonstrated to be accurate, robust and sensitive for the determination of dimethyl sulfate impurity in methoxsalen drug substance.

scholarly journals Chemical Characterization of Electronic Cigarette (e-cigs) Refill Liquids Prior to EU Tobacco Product Directive Adoption: Evaluation of BTEX Contamination by HS-SPME-GC-MS and Identification of Flavoring Additives by GC-MS-O

Atmosphere ◽  
2020 ◽  
Vol 11 (4) ◽  
pp. 374
Author(s):  
Jolanda Palmisani ◽  
Carmelo Abenavoli ◽  
Marco Famele ◽  
Alessia Di Gilio ◽  
Laura Palmieri ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase ◽  
Tobacco Product ◽  
Gas Chromatography Mass Spectrometry ◽  
Contamination Level ◽  
The European Union ◽  
Limit Of Quantification ◽  
Chromatography Mass Spectrometry ◽  
Concentration Levels

The present study focused on the determination of benzene, toluene, ethylbenzene and xylenes (BTEX) concentration levels in 97 refill liquids for e-cigs selected by the Italian National Institute of Health as representative of the EU market between 2013 and 2015 prior to the implementation of the European Union (EU) Tobacco Product Directive (TPD). Most of the e-liquids investigated (85/97) were affected by BTEX contamination, with few exceptions observed (levels below the limit of quantification (LOQ) of headspace-solid phase micro extraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) methodology). Across brands, concentration levels ranged from 2.7 to 30,200.0 µg/L for benzene, from 1.9 to 447.8 µg/L for ethylbenzene, from 1.9 to 1,648.4 µg/L for toluene and from 1.7 to 574.2 µg/L for m,p,o-xylenes. The variability observed in BTEX levels is likely to be related to the variability in contamination level of both propylene glycol and glycerol and flavoring additives included. No correlation was found with nicotine content. Moreover, on a limited number of e-liquids, gas chromatography-mass spectrometry-olfactometry (GC-MS-O) analysis was performed, allowing the identification of key flavoring additives responsible of specific flavor notes. Among them, diacetyl is a flavoring additive of concern for potential toxicity when directly inhaled into human airways. The data reported are eligible to be included in the pre-TPD database and may represent a reference for the ongoing evaluation on e-liquids safety and quality under the current EU Legislation.

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