Identification of endogenous metabolites in human sperm cells using proton nuclear magnetic resonance (1H-NMR) spectroscopy and gas chromatography-mass spectrometry (GC-MS)

Andrology ◽  
2015 ◽  
Vol 3 (3) ◽  
pp. 496-505 ◽  
Author(s):  
C. Paiva ◽  
A. Amaral ◽  
M. Rodriguez ◽  
N. Canyellas ◽  
X. Correig ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Gas Chromatography ◽  
Nmr Spectroscopy ◽  
1H Nmr Spectroscopy ◽  
Human Sperm ◽  
Proton Nuclear Magnetic Resonance ◽  
Gas Chromatography Mass Spectrometry ◽  
Sperm Cells ◽  
Endogenous Metabolites

Comparison of hydrogenolysis with thioacidolysis for lignin structural analysis

Holzforschung ◽  
2014 ◽  
Vol 68 (2) ◽  
pp. 151-155 ◽  
Author(s):  
Daniel J. van de Pas ◽  
Bernadette Nanayakkara ◽  
Ian D. Suckling ◽  
Kirk M. Torr
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Gas Chromatography ◽  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Magnetic Resonance ◽  
Gas Chromatography Mass Spectrometry ◽  
Aryl Ether ◽  
Chromatography Mass Spectrometry

Abstract Mild hydrogenolysis has been compared with thioacidolysis as a method for degrading lignins in situ and in isolated form before analysis by gas chromatography/mass spectrometry and quantitative 31P nuclear magnetic resonance (NMR) spectroscopy. Both degradation methods gave similar levels of β-aryl ether-linked phenylpropane units that were released as monomers. Degradation by hydrogenolysis generally gave lower levels of total phenylpropane units when analyzed by 31P NMR, especially in the case of lignins with high levels of condensed units. Overall, these results indicate that mild hydrogenolysis could offer an alternative to thioacidolysis for probing lignin structure.

scholarly journals An Optimization of Liquid–Liquid Extraction of Urinary Volatile and Semi-Volatile Compounds and Its Application for Gas Chromatography-Mass Spectrometry and Proton Nuclear Magnetic Resonance Spectroscopy

Molecules ◽  
2020 ◽  
Vol 25 (16) ◽  
pp. 3651
Author(s):  
Natalia Drabińska ◽  
Piotr Młynarz ◽  
Ben de Lacy Costello ◽  
Peter Jones ◽  
Karolina Mielko ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Gas Chromatography ◽  
1H Nmr ◽  
Biomarker Discovery ◽  
Liquid Extraction ◽  
Proton Nuclear Magnetic Resonance ◽  
Gas Chromatography Mass Spectrometry ◽  
Resonance Spectroscopy ◽  
Liquid Liquid Extraction

Urinary volatile compounds (VCs) have been recently assessed for disease diagnoses. They belong to very diverse chemical classes, and they are characterized by different volatilities, polarities and concentrations, complicating their analysis via a single analytical procedure. There remains a need for better, lower-cost methods for VC biomarker discovery. Thus, there is a strong need for alternative methods, enabling the detection of a broader range of VCs. Therefore, the main aim of this study was to optimize a simple and reliable liquid–liquid extraction (LLE) procedure for the analysis of VCs in urine using gas chromatography-mass spectrometry (GC-MS), in order to obtain the maximum number of responses. Extraction parameters such as pH, type of solvent and ionic strength were optimized. Moreover, the same extracts were analyzed using Proton Nuclear Magnetic Resonance Spectroscopy (1H-NMR), to evaluate the applicability of a single urine extraction for multiplatform purposes. After the evaluation of experimental conditions, an LLE protocol using 2 mL of urine in the presence of 2 mL of 1 M sulfuric acid and sodium sulphate extracted with dichloromethane was found to be optimal. The optimized method was validated with the external standards and was found to be precise and linear, and allowed for detection of >400 peaks in a single run present in at least 50% of six samples—considerably more than the number of peaks detected by solid-phase microextracton fiber pre-concentration-GC-MS (328 ± 6 vs. 234 ± 4). 1H-NMR spectroscopy of the polar and non-polar extracts extended the range to >40 more (mainly low volatility compounds) metabolites (non-destructively), the majority of which were different from GC-MS. The more peaks detectable, the greater the opportunity of assessing a fingerprint of several compounds to aid biomarker discovery. In summary, we have successfully demonstrated the potential of LLE as a cheap and simple alternative for the analysis of VCs in urine, and for the first time the applicability of a single urine solvent extraction procedure for detecting a wide range of analytes using both GC-MS and 1H-NMR analysis to enhance putative biomarker detection. The proposed method will simplify the transport between laboratories and storage of samples, as compared to intact urine samples.

scholarly journals Metabolomic Profiling of Human Spermatozoa in Idiopathic Asthenozoospermia Patients Using Gas Chromatography-Mass Spectrometry

2018 ◽  
Vol 2018 ◽  
pp. 1-8 ◽  
Author(s):  
Kai Zhao ◽  
Jianzhong Zhang ◽  
Zhen Xu ◽  
Yue Xu ◽  
Aiming Xu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Krebs Cycle ◽  
Human Sperm ◽  
Gas Chromatography Mass Spectrometry ◽  
Sperm Cells ◽  
Spectrometric Data ◽  
Metabolomic Profiling ◽  
Chromatography Mass Spectrometry ◽  
First Time

The purpose of this study was to describe the first metabolic profile of human sperm cells through the application of an untargeted platform based on gas chromatography-mass spectrometry (GC-MS). Sperm cell samples from patients diagnosed with idiopathic asthenozoospermia (n=30) and healthy subjects (n=30) were analyzed using a nontargeted metabolomics method based on GC-MS spectroscopy. The mass spectrometric data were collected using multivariate and univariate analyses to identify metabolites related to idiopathic asthenozoospermia. By using metabolomic strategies, we identified 33 metabolites, 27 of which were decreased in the idiopathic asthenozoospermia group compared with the normozoospermic group and six were increased in idiopathic asthenozoospermia. With respect to human sperm cells, some of these metabolites are reported here for the first time. Pathways for nucleoside, amino acid and energy metabolism, and the Krebs cycle were disturbed and were associated with idiopathic asthenozoospermia. The metabolic profiling provides an important first step in studying the pathophysiological mechanisms involved in IAS, and the identified metabolites may become potential biomarkers for its diagnosis and treatment.

Use of high-resolution proton nuclear magnetic resonance spectroscopy for rapid multi-component analysis of urine.

1984 ◽  
Vol 30 (3) ◽  
pp. 426-432 ◽  
Author(s):  
J R Bales ◽  
D P Higham ◽  
I Howe ◽  
J K Nicholson ◽  
P J Sadler
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Magnetic Resonance ◽  
High Resolution ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Proton Nuclear Magnetic Resonance ◽  
Resonance Spectroscopy ◽  
Simple Method ◽  
Nuclear Magnetic

Abstract Numerous low-Mr metabolites--including creatinine, citrate, hippurate, glucose, ketone bodies, and various amino acids--have been identified in 400- and 500-MHz proton nuclear magnetic resonance (1H NMR) spectra of intact human urine. The presence of many of these was related to the specific condition of the donors: humans in different physiological states (resting, fasting, or post-exercise) and pathological conditions (e.g., diabetes mellitus, cadmium-induced renal dysfunction). We have also monitored the metabolism of simple nonendogenous compounds (methanol and ethanol) and of acetaminophen. The pH-dependencies of the NMR chemical shifts of some urine components are reported. Our studies show that high-resolution 1H NMR spectroscopy provides a fast, simple method for "fingerprint" identification of urinary compounds. In some cases, analytes can be quantified by standard additions or by comparing integrated peak areas for the metabolites with those for creatinine. Determinations of creatinine by 1H NMR spectroscopy compared well with those by an independent chemical assay based on the Jaffé reaction.

scholarly journals Chemical Composition of Needle, Cone, and Branch Oils From Vietnamese Pinus cernua

2019 ◽  
Vol 14 (5) ◽  
pp. 1934578X1985099 ◽  
Author(s):  
Tran Hui Thai ◽  
Nguyen Thi Hien ◽  
Le Ngoc Diep ◽  
Mathieu Paoli ◽  
Joseph Casanova ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Gas Chromatography ◽  
Chemical Composition ◽  
Magnetic Resonance ◽  
Retention Index ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Main Component ◽  
Pine Species

Conifers are well represented in Vietnam where a new pine species has been recently discovered in Son La province: Pinus cernua, synonym P. armandii ssp. xuannhaensis. The compositions of needle, cone, and branch oils have been investigated by gas chromatography (retention index), gas chromatography-mass spectrometry, and 13C nuclear magnetic resonance. Myrcene (47.0%) was the main component of needle oil, followed by β-pinene (28.4%) and α-pinene (12.5%). Branch oil also contained myrcene (32.8%), α-pinene (17.9%), β-pinene (9.8%), and a high content of limonene (20.0%). Finally, cone oil displayed α-pinene (44.1%) beside myrcene (11.5%), β-pinene (8.1%), and limonene (5.8%).

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