Mass Spectrometry

Ilgar Mamedov completed his PhD and Postdoctoral studies in Pirogov Russian National Research Medical University (RNRMU). He has worked as Scientific Worker in Science Research and Clinical Institute for Pediatrics (Moscow, Russia). He has published more than 20 papers in reputed journals and has been serving as Director for innovation at LLC ChromsystemsLab in Moscow (Russia).

Long chain fatty acids as well as the fatty acids with a branched chain, pristanic and phytanic acid, are extremely hydrophobic and practically insoluble in water. Inside the cell, they are in the form of esters of coenzyme A. In patients with abnormal peroxisome function, an increased content long chain fatty acids chain longer than 26 carbon atoms will be observed in the process of diagnosis can also use fatty acid: hexacosanoic acid C26:0, lignoceric acid C24:0, behenic acid C22:0, and their relations. In our work, we used the method of gas chromatography with mass detection (GC-MS) and electron impact ionization (Shimadzu GCMS QP-5050A). The method involves the preliminary derivatization of N-methyl-N(tert-butyldimethylsilyl)triflyuoroacetamide (MTBSTFA). In order to determine the total content long chain fatty acids, pristanic and phytanic acid samples should be subjected to acid and alkaline hydrolysis followed by extraction with hexane. The reference values were defined as confidence interval 2.5-97.5% spread in the control group. Reference values of unbranched fatty acids used in this paper were obtained by analyzing 168 control samples by GC/MS. Long chain fatty acids concentration in control samples is independent of age. Pathological values may differ for different inherited disorders peroxisomal functions. It is essential to link the cases with the maximum number peroxisome functions. The procedure of the analysis of long chain fatty acids by gas chromatography of the sample preparation step was investigated to obtain a specific result. Presented with reference values basic levels of long chain fatty acids and main biochemical markers in plasma in children and adult.

Petra Bursíková has completed her PhD in Fire Protection from Technical University of Ostrava in Czech Republic. Both have been working at Fire Technical Institute in research team. The focus is on the using analytical method for the investigation of fire cause.

The fire-technical expertise in the field of fire detection is a highly sophisticated analysis of all available information related to the fire. By evaluating all the information and knowledge, one of the possible versions of the causes of a fire can be confirmed, and often can explain a course and spread of fire. Except for information from a fire scene, photographic and technical documentation, the facts about substances and materials found in the fire focus and its surroundings in terms of chemical composition and presence of flammable substances must be known. The analytical methods used in the Technical Institute of Fire Protection for identifying a substance of an unknown substance from a fire scene, either for a solid, liquid or gaseous mixture, are as follows: gas chromatography, X-ray fluorescence spectroscopy, Fourier transforms infrared (spectroscopy), Raman spectroscopy and optical emission spectrometry. Gas chromatography is able to confirm the presence of small amounts of organic matter trapped in solid samples from fires. Analysis of volatile substances is widely used to demonstrate the presence of traces of combustible liquids used as substances supporting flame (flame accelerants). The presence of gasoline or diesel fuel traces can significantly support the hypothesis of intentional fire. FTIR and Raman spectroscopy can be used to determine the molecular composition of an unknown sample. The methods are especially suitable for the identification of organic and inorganic substances, plastics, paints, building and construction materials. We can use X-ray fluorescence analysis method to determine elemental composition of inorganic materials in solid and liquid state, e.g. in metallic alloys, ash or carbonaceous residues. The analysis of the elements is supplemented by the classical elemental analysis performed on the elemental analyzer to determine the representation of carbon, hydrogen and nitrogen elements. Using optical emission spectrometry, it is possible to determine the exact composition of an unknown metal alloy found on a fire scene.

Velikanova L I completed her PhD and has got the Doctorate in Biological Science (Russian Doctor of Science Degree) from North-Western State Medical University (NWSMU) named after I I Mechnikov, Saint-Petersburg, Russian Federation. She is the Head of Research Laboratory of Chromatography in NWSMU. Her area of interests includes teroidogenesis, adrenal diseases, HPLC and GC-MS. She has published more than 50 papers in Russian and foreign journals.

Determination of steroids and their metabolites in urine by gas chromatography with mass-spectrometric detection (GC–MS) is a powerful diagnostic tool in the study of adrenal diseases. Sample preparation conditions (hydrolysis, extraction, derivatization) and chromatographic separation of 66 steroids (androgens, glucocorticoids, mineralocorticoids and their precursors) were optimized. We analyzed urinary steroid profiles (USP) in 29 obese patients (OB), 45 patients with Cushing’s syndrome (CS), 28 patients with Cushing’s disease (CD), 16 patients with malignant corticosteroma (MC) and 27 healthy people. USP were performed on a gas chromatograph-mass spectrometer SHIMADZU GCMS-QP2010 ULTRA. OB patients had increased urinary excretion of androgens [androsterone (An), 11-OH-An, androstenediole-17β (17βdA2)], glucocorticoids [allo-tatrahydrocortisol (allo-THF), allo-tetrahydrocorticosterone (allo-THB), tetrahydro-11-dehydrocorticosterone (THA) and cortolones]. Increased allo-THF/5β-THF, allo-THB/THB and 11-ОНAn/11-ОН-Et ratios may indicate an increase of 5α-reductase activity, a depression of ТНF/THE and ТНВ/ТНА ratios indicated a decrease of 11β-hydroxysteroiddehydrogenase (11β-НSDH) type I activity in OB patients. Patients with CS and CD had increased excretion of the following glucocorticoids: tetrahydro11-deoxycortisol (THS), THE, 5β-THF, 5β-THB, cortolones, cortols, dihydrocortisone and dihydrocortisol. Decrease of urinary excretion of An, etiocholanolone (Et), dehydroepiandrosterone (DHEA) and androstentriole (dA3) had patients with CS, increased urinary excretion of androgens had patients with CD. Patients with MC received 2 USP types by GC-MS. Common features of MC were increasing urinary excretion of THS (>1500 µg/24 h), pregnantriol (P3), 11-oxo-P3, pregnendiol (DP2) pregnentriol (DP3), 16-OHDP2, 16-OHDP2-3β, DP3-3β, 16-OH-pregnenolone (16dP), 21dP, 11DP3. Additional features of ACC in 6 MC patients (type 2) increased urinary excretion of DHEA (>2500 µg/24 h) and its metabolites (17βdA2, 16-OHDEA, 16-oxo-dA2, dA3). A decrease of An/Еt and allo-THF/5β-THF ratios may indicate an increase of 5β-reductase activity, increased ТНF/THE, (ТНF+alloTHF)/THE, (ТНF+allo-THF+cortols)/(THE+allo-THE+cortolones) and ТНВ/ТНА ratios may indicate the decreasing of 11β-НSDH type II activity in patients with CS and MC

Saif S Abbas is pursuing his Master’s Degree in Pharmaceutics/Pharmacokinetics in Al-Ahliyya Amman University in Jordan. He graduated from the Faculty of Pharmacy and Medical Sciences in Al-Ahliyya Amman University, Jordan in 2013. He has worked as a Senior Pharmacist in retail pharmacies and drug stores in Amman, Jordan.

Ivabradine is a new hyperpolarization-activated cyclic nucleotidegated channel blocker. It has been approved by the FDA in 2015 in management of stable angina and congestive heart failure. The aim of this study was to investigate the possibility of pharmacokinetic interaction of a proposed combination of ivabradine and the β-blocker carvedilol in rats using spectroscopy technique. A simple, rapid and sensitive method for validation and determination of ivabradine and carvedilol in the ratsʼ plasma was developed using HPLC/MS. The method was successfully developed and validated in terms of linearity, precision and accuracy which were within the values accepted by EMEA and ICH. Ivabradine and carvedilol were given both intravenously and orally, each alone and as oral combination to fasting Sprague-Dawley rats. Blood samples were withdrawn on scheduled time intervals up to 36 hours and analyzed for each drug. Both compartmental and non-compartmental kinetic analyses were performed on plasma level-time data and the kinetic parameters were calculated from non-compartmental analysis. Results showed significant increase in bioavailability of both drugs in combination (94% for carvedilol and 58% for ivabradine. Also, Cmax was changed significantly by 165% for carvedilol and 56% for ivabradine, when given in combination. There was also a significant decrease in elimination of both drugs expressed as 48% decrease in clearance and 41% increase in the half-life for carvedilol and 32% decrease in clearance and 37% increase of the half-life of ivabradine when given in combination. These changes suggested an interaction on metabolic function of the liver on both drugs by some kind of enzyme inhibition. Also, the rate of absorption of ivabradine was slowed by concomitant administration of carvedilol suggesting an interaction on absorption level. In conclusion, a significant kinetic interaction occurred when ivabradine was given orally with carvedilol which makes dose adjustment of both drugs of much importance.

Eman Farouk Ahmed Mohamed has graduated from Faculty of Science, University of Alexandria. She has completed Diploma in Analytical Chemistry and then completed her Master’s degree in Organic Chemistry from Institute of Graduate Studies and Research Alexandria University. She is currently working as Chemist analyzing pesticide residues in water lab in Central Laboratories of Alexandria (CLA), Ministry of Health, Egypt

The environmental pollution with pesticides and other organic contaminants initiated the interest to investigate the level and the fate of these compounds in different environmental compartments. Contamination of water resources by pesticide residues is one of the major challenges for the preservation and sustainability of the environment. However, these pesticides must be used properly, abiding by the law, the environment and human health, since they are toxic and can cause contamination. In Egypt, the use of organochlorine insecticides began in the 1950s. DDT, endrin and other organochlorine pesticides were extensively used until 1981. This class of chemicals is characterized by their long persistence in the environment. The organic contaminants (e.g. OCPs) in environmental samples are often affected by sample matrix constituents who may interfere with the chromatographic separation of contaminants and lead to misidentification of chromatographic peaks and wrong quantification. The class of pesticides is scarce; the majority of matrix effects are promoted by the complex chemical composition of the environmental matrix, especially changes in physicochemical characterization such as pH, turbidity, suspension and electrical conductivity (EC). In our study we extracted water samples according to EPA 508.1. The results showed positive differences for the levels of pesticide residues between water types like industrial wastewater and drinking water. We also found that physicochemical parameters measured in types of water effect on the efficiency of pesticides recovery percentages was (ranged from 74.54% to 99.5%). For further work, we will study different types of water like drainage wastewater, municipal wastewater, sea wastewater, etc. to investigate the relation between physicochemical characterization on pesticides residuals analysis. Assessing the recovery efficiency and detection limits of the parameters will be measured are tools to specify the sensitive and accuracy of the qualitative and quantitative analysis by mass spectrometry

Romana Friedrichová has completed her PhD in Chemistry and Technology of Materials from the University of Chemistry and Technology, Prague in Czech Republic. The focus is on the using analytical method for the investigation of fire cause

The fire-technical expertise in the field of fire detection is a highly sophisticated analysis of all available information related to the fire. By evaluating all the information and knowledge, one of the possible versions of the causes of a fire can be confirmed, and often can explain a course and spread of fire. Except for information from a fire scene, photographic and technical documentation, the facts about substances and materials found in the fire focus and its surroundings in terms of chemical composition and presence of flammable substances must be known. The analytical methods used in the Technical Institute of Fire Protection for identifying a substance of an unknown substance from a fire scene, either for a solid, liquid or gaseous mixture, are as follows: gas chromatography, X-ray fluorescence spectroscopy, Fourier transforms infrared (spectroscopy), Raman spectroscopy and optical emission spectrometry. Gas chromatography is able to confirm the presence of small amounts of organic matter trapped in solid samples from fires. Analysis of volatile substances is widely used to demonstrate the presence of traces of combustible liquids used as substances supporting flame (flame accelerants). The presence of gasoline or diesel fuel traces can significantly support the hypothesis of intentional fire. FTIR and Raman spectroscopy can be used to determine the molecular composition of an unknown sample. The methods are especially suitable for the identification of organic and inorganic substances, plastics, paints, building and construction materials. We can use X-ray fluorescence analysis method to determine elemental composition of inorganic materials in solid and liquid state, e.g. in metallic alloys, ash or carbonaceous residues. The analysis of the elements is supplemented by the classical elemental analysis performed on the elemental analyzer to determine the representation of carbon, hydrogen and nitrogen elements. Using optical emission spectrometry, it is possible to determine the exact composition of an unknown metal alloy found on a fire scene.