scholarly journals A Single LC-MS/MS Analysis to Quantify CoA Biosynthetic Intermediates and Short-Chain Acyl CoAs

Metabolites ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 468
Author(s):  
Anthony E. Jones ◽  
Nataly J. Arias ◽  
Aracely Acevedo ◽  
Srinivasa T. Reddy ◽  
Ajit S. Divakaruni ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Sample Preparation ◽  
Biosynthetic Pathway ◽  
Solid Phase ◽  
High Sensitivity ◽  
Short Chain ◽  
Extraction Column ◽  
Chain Acyl ◽  
Precision And Accuracy ◽  
Mass Spectrometry Mass Spectrometry

Coenzyme A (CoA) is an essential cofactor for dozens of reactions in intermediary metabolism. Dysregulation of CoA synthesis or acyl CoA metabolism can result in metabolic or neurodegenerative disease. Although several methods use liquid chromatography coupled with mass spectrometry/mass spectrometry (LC-MS/MS) to quantify acyl CoA levels in biological samples, few allow for simultaneous measurement of intermediates in the CoA biosynthetic pathway. Here we describe a simple sample preparation and LC-MS/MS method that can measure both short-chain acyl CoAs and biosynthetic precursors of CoA. The method does not require use of a solid phase extraction column during sample preparation and exhibits high sensitivity, precision, and accuracy. It reproduces expected changes from known effectors of cellular CoA homeostasis and helps clarify the mechanism by which excess concentrations of etomoxir reduce intracellular CoA levels.

scholarly journals Neonatal Screening on Tandem Mass Spectrometry as a Powerful Tool for the Reassessment of the Prevalence of Underestimated Diseases in Newborns and Their Family Members: A Focus on Short Chain Acyl-CoA Dehydrogenase Deficiency

2020 ◽  
Vol 6 (3) ◽  
pp. 58
Author(s):  
MariaAnna Messina ◽  
Alessia Arena ◽  
Agata Fiumara ◽  
Riccardo Iacobacci ◽  
Concetta Meli ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Newborn Screening ◽  
Dehydrogenase Deficiency ◽  
Family Members ◽  
Clinical Manifestations ◽  
Vitamin B12 Deficiency ◽  
Short Chain ◽  
Tandem Mass ◽  
Chain Acyl

Early detection of disabling diseases, prior to clinical manifestations, is the primary goal of newborn screening (NS). Indeed, the required number of core and secondary conditions selected for screening panels is increasing in many countries. Furthermore, newborn screening can lead to diagnosis of maternal diseases such as vitamin B12 deficiency or 3-MethylcrotonylCoA-carboxylase deficiency (3MCC). NS became mandatory in Sicily in December 2017. Here we report NS data collected between December 2017 and April 2020. Our results show that tandem mass spectrometry is a powerful tool for discovery of underestimated disease in newborns and their family members. Our panel included short chain acyl-CoA dehydrogenase deficiency (SCADD). Here, we report that results of our investigation led to reassessment of SCADD prevalence in our population. The infant and adult patients diagnosed in our study had previously not shown overt symptoms.

scholarly journals Headspace Solid-Phase Microextraction Coupled to Comprehensive Two-Dimensional Gas Chromatography Time-of-Flight Mass Spectrometry for the Determination of Short-Chain Chlorinated Paraffins in Water Samples

2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Nan Zhan ◽  
Feng Guo ◽  
Shuai Zhu ◽  
Zhu Rao
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Water Samples ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Short Chain ◽  
Two Dimensional ◽  
Flight Mass Spectrometry ◽  
Chlorinated Paraffins

Short-chain chlorinated paraffins (SCCPs) are a new type of persistent organic pollutants. In this work, a simple and effective method involving headspace solid-phase microextraction (HS-SPME) and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOF-MS) was developed and optimized for the determination of trace SCCPs in water samples. The key parameters related to extraction and separation efficiency were systematically optimized. The SCCP congener groups were best resolved using an Rxi-5Sil MS (30 m × 0.25 mm × 0.25 µm) column followed by an Rxi-17Sil MS (1.0 m × 0.15 mm × 0.15 µm) column; the optimum extraction conditions were achieved with a 100 µm polydimethylsiloxane SPME fiber, when a 10 mL water sample added with 3.6 g sodium chloride was incubated for 15 min at 90°C and then extracted during 60 min at 90°C and desorption at 260°C for 2 min. The proposed method showed good linearity in the concentration range of 0.2–20.0 µg/L with the determination coefficient greater than 0.995. The detection and quantification limits ranged from 0.06 to 0.13 µg/L and 0.18 to 0.40 µg/L, respectively, which are sufficient to meet the regulatory detection limits as set by most environmental regulations. The accuracy and precision of the method was also good, where the recoveries ranged from 82.5 to 95.4%, and intra- and interday precision was within 7.2% and 14.5%, respectively. The optimized method has been applied to the determination of SCCPs in ten freshwater samples of three different types.

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 Determination of 24 Pesticides Residues in Leather Products by Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry

2020 ◽  
Vol 20 (4) ◽  
pp. 385-404
Author(s):  
Jinlan DAI ◽  
Honglei YIN ◽  
Hang WEI ◽  
Lei ZHOU ◽  
Minghua LIU
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Extraction Column ◽  
Phase Extraction ◽  
Mixed Solution ◽  
Pesticides Residues ◽  
Solid Phase Extraction Column ◽  
Relative Standard

Considering the high content of oil and complex residual additives in leather samples, a new analytical method based on the solid-phase extraction technique and gas chromatography-selected ion monitoring mass spectrometry (GC-SIM-MS) was developed to determine 24 organic compounds involving the organochlorine pesticides (OCPs), organophosphorous pesticides (OPPs) and pyrethroids pesticides residues in leather. The extraction conditions (such as the extraction solution, purification procedure and solid-phase extraction column) were optimized using the positive leather samples based on the recovery rates of the pesticides. The best extraction solution, solid-phase extraction column and chromatography column were n-hexane and ethyl acetate (1+1, volume) mixed solution, Carb-PSA (1.0 g, 6mL) and DB-1701 (length: 30 m, inside diameter: 0.25 mm, film thickness: 0.25 μm). The optimized extraction time and temperature were 20 min and 25°C, respectively. The detection limits of 24 pesticide residues range from 0.05 to 0.10 mg/kg, and the recoveries range from 74% to 116%. The relative standard deviations (RSD, n=6) range from 5.42% to 12.00%. The developed method presented a simple, rapid, sensitive, and inexpensive method to detect 24 pesticides in skin and leather and was successfully applied to the detect them in leather products (cowhide, sheep leather and pig leather).

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