A comparative mass spectrometric study of fatty acids and metals in some seed extracts.

A major cause of cardiovascular diseases and cancer is diet content, so the optimization of micronutrients in food is very important. Omega-3 fatty acids supplementation for patients had beneficial effects on subjective global assessment score and metabolic profiles. Fatty acids content and the metal ions in different seeds (e.g. linseed, poppy, grape, hemp, nuts, pumpkin, sesame, watermelon, chia) recommended as food supplements, purchased on the Romanian market, were compared. Gas chromatography coupled to mass spectrometry (GC-MS) was used as an excellent technique for fatty acids identification and quantitation, and inductively coupled plasma mass spectrometer (ICP-MS) for analytical measurements of metals.

Evaluation of discriminant functions for sexing skulls from visually assessed traits applied in the Rainer Osteological Collection (Bucharest, Romania).

The sexing of human skeletal remains based on visual scoring of descriptive traits on the skull is useful for both forensic and bioarchaeological studies, given that many such features preserve well in the field and can be assessed quickly. The goal of our work is to evaluate the accuracy of this method on an age-balanced, known sex, random sample of 360 modern adult crania in the Rainer Osteological Collection. Consistent with Walker (2008), we scored glabella area (G), the mastoid process (Ma), the mental eminence (M), the orbital edge (O) and the nuchal crest (N), on a five-point scale. We generated sex discriminant functions (logistic), selected the most accurate of them, and subsequently applied them to archaeological samples from Romania. Each skull feature showed significant score differences by sex. Eight out of 31 discriminant functions passed criteria of high accuracy (∼90%), sex bias (±2%), and ease of use (direct calculation of sex). The best estimates were obtained for the 30-60 age groups. Further testing these functions on six archaeological samples showed high percentages of agreement with the sex assessed on the coxal bone. The study also indicated that, although easy to learn by novices, the method of visually scoring the skull traits depends on prior experience with human osteology. The accuracy of the method may be influenced by geographical and historical differences which are bound to exist between populations.

Dinuclear manganese centers in the manganese-lead-tellurate glasses.

FTIR, UV-VIS and EPR spectra of manganese doped lead-tellurate glasses with composition xMnO·(100-x)[4TeO2·PbO2] where x=0, 1, 5, 10, 20, 30, 40mol% have been studied. The FTIR spectra show the formation of the Mn-O-Pb and Mn-O-Te bridging bonds by increasing of MnO concentration. The UV-VIS spectra show the Mn(+3) species exhibit pronounced absorption, which masks the Mn(+2) spin-forbidden absorption bands when Mn(+2) ions are in high concentrations in these glasses. The EPR spectra exhibit resonance signals characteristic of Mn(+2) ions. The resonance signal located at g≈2 is due to Mn(+2) ions in an environment close to octahedral symmetry, whereas the resonance at g≈4.3 and 3.3 are attributed to the rhombic surroundings of the Mn(+2) ions. The increase in the MnO content gives rise to absorption at g≈2.4 and the paramagnetic ions are involved in dinuclear manganese centers.

Dual role of the six-coordinated molybdenum and lead ions in novel of photochromic properties of the molybdenum-lead-borate glasses.

Transparent glasses were prepared by conventional melting-quenching method in the xMoO(3).(100-x)[3B(2)O(3).PbO] system where 0

Toward modeling phosphate tellurate glasses: the devitrification and addition of gadolinium ions behavior.

Glasses in the xGd2O3 x (100 - x)[7TeO2 x 3P2O5] system with 0 < or = x < or = 20 mol % have been prepared using the melt quenching method. The influence of gadolinium ions on structural behavior of the phosphate tellurate glass has been investigated using infrared spectroscopy and density functional theory (DFT) calculations. The addition of gadolinium ions into the host glass matrix leads to an increase of the glass network polymerization due to the replacement of P-O-P bonds by the more resistant P-O-Te bonds having as result the improvement of the chemical durability of the glass. The structural evolution of the studied glasses with the gradual increase of the gadolinium oxide content up to 20 mol % could be explained by considering that the excess of oxygen may be accommodated by the conversion of some orthophosphate structural units into metaphosphate or/and pyrophosphate units. X-ray diffraction and IR spectra revealed that heat treatment of the samples also causes an increase of the glass network polymerization for heat treatment times, t, up to 36 h, while for 36 h > t > or = 48 h showed a drastic structural modification which lead to the apparition of the Te4P2O13 crystalline phase. DFT calculations show that tellurium atoms occupy two different sites in the proposed model. In the first case the tellurium atom is coordinated with four oxygen atoms giving a trigonal bipyramide arrangement, while in the second case the tellurium atom is coordinated with three O atoms. The calculated IR absorption spectrum of the proposed model for phosphotellurite glasses is in good agreement with the experimental absorption data.

Reliability of salivary theophylline in monitoring the treatment for apnoea of prematurity.

OBJECTIVE: To evaluate the reliability of salivary levels of theophylline in monitoring therapy of apnoea of prematurity. STUDY DESIGN: Aminophylline was administered intravenously in 13 infants with apnoea, in a loading dose of 5 mg/kg and maintenance dose of 3 mg/kg, every 8 h. The patients were divided into two groups according to their postconceptional age (PCA): group A, of infants with small PCA (32.8+/-2.0 weeks; n=6 cases), and group B, infants with higher PCA (37.1+/-0.8 weeks; n=7 cases). RESULTS: A total of 57 paired samples of serum and saliva were obtained in all 13 infants. The mean serum level of theophylline was 7.8+/-5.8 microg/ml and the ratio between serum and salivary concentration of theophylline was 1.53+/-0.28. A strong correlation between the serum and salivary concentration of theophylline (r=0.973) was found. Infants with small PCA had significant higher serum concentration of theophylline than those with higher PCA (10.6 vs 5.3 microg/ml; P=0.0002). The difference between the mean ratios of serum/salivary theophylline levels in the two groups was low (1.44 vs 1.62; P=0.0155). CONCLUSION: The strong correlation of theophylline in serum and in saliva recommends the salivary levels as a reliable method for monitoring the treatment of apnoea of prematurity.

Electron impact mass spectral interpretation for some thiophosphoryl-p-acetylaminobenzenesulfonamides.

This work discusses the synthesis and the fragmentation patterns for 2-(p-acetylaminosulfonamido)-2-thiono-(5,5-dimethyl-1,3,2-dioxaphosphorinane)(1) and for the p-acetylaminosulfonylamides of O,O-diethylthiophosphoric acid (2), O,O-diphenylthiophosphoric acid (3), dimethylaminocyclohexylthiophosphoric acid (4), and diethylaminophenylthiophosphoric acid (5). A thionamidic-thiolimidic structure was attributed to compounds 1-5, consistent with their IR and NMR spectra. EI mass spectra at 70 eV, high resolution (HR) mass measurements and metastable ion spectra were used to elucidate the fragmentation processes and to determine the kinetic energy release values associated with the metastable ion dissociations. HR accurate mass measurements were used to confirm the compositions of the more abundant ions.

Comparative analysis of some active principles of herb plants by GC/MS.

A rapid extraction procedure for fingerprint chromatogram of different types of Mentha piperita L. (Labiatae family) is presented. The extracts were analysed by gas chromatography and gas chromatography-mass spectrometry (GC/MS). The main volatile compounds identified by the gas chromatography-mass spectrometric analysis of M. piperita L. were menthol, menthone, isomenthone, 1,8-cineole, menthyl acetate, limonene, beta-myrcene, carvone. M. piperita L. oil had the active principles: menthol, menthone, isomenthone, menthyl acetate, alpha-pinene, beta-pinene, champhor, limonene, linalool, piperitone. M. crispa L. showed carvone as major component.

[The monitoring of delayed-release theophylline therapy in bronchial asthma in children by determining the salivary concentration]. / Monitorizarea terapiei cu teofilina cu eliberare întârziata în astmul bronsic la copil prin determinarea concentratiei salivare.

Long-term therapy with slow-release theophylline is compulsory to be monitorized by measuring serum concentration of the drug. This is due to the narrow therapeutically index of theophylline for monitoring the long term therapy with this drug, and to establish the correlation between the serum and saliva concentration of theophylline. The study group was represented by 13 children with asthma, with the age between 2 and 13 years that received theophylline in an average dosage of 15.2 mg/kg/24 hours. In all of them there were obtained two paired simultaneous samples of venous blood and of saliva, at 4 hours and at 8 hours respectively, after the administration of theophylline. For facilitate the saliva sampling, its production was stimulated by applying citric acid on the tongue and aspiration with a sterile syringe. For measuring the serum and saliva levels of the drug it was used mass spectrometry with 15N-theophylline as internal standard. Serum theophylline concentration varied between 6.56 +/- 4.48 micrograms/ml at 8 hours after drug administration and respectively 7.45 +/- 3.94 micrograms/ml at 4 hours after drug administration. Saliva concentrations of theophylline varied between 4.18 +/- 2.40 micrograms/ml at 8 hours after drug administration and respectively 4.66 +/- 2.39 micrograms/ml at 4 hours after drug administration. The average ratio between serum and saliva concentration in the 24 paired samples was 1.62 +/- 0.18. The intraindividual variation of this ratio was 8.64%.

Separation, identification and quantitative determination of free amino acids from plant extracts.

This research presents the results obtained from the separation, identification and quantitative determination of free amino acids from Gingko biloba and Hedera helix leaf extracts, using three modern techniques: thin layer chromatography (TLC), high performance liquid chromatography (HPLC), and gas chromatography-mass spectrometry. The presence of the determined amino acids explains the utilisation of G. biloba and H. helix leaf extracts in cosmetic and pharmaceutical products.

[The evaluation parameters of the long-term treatment efficacy of theophylline in the child with bronchial asthma]. / Parametrii de evaluare a eficientei tratamentului de durata cu teofilina la copilul cu astm bronsic.

In the past decade the use of theophylline was less extensive because of its narrow therapeutically index and due to its side effects. The widening of possibilities of monitoring the treatment by serum level determination, the introduction of slow release formula, and the demonstration of antiinflammatory effects made theophylline to become actual again. Theophylline is indicated for the chronic treatment of asthma in association with other medication. The authors study the efficacy and serum level of theophylline in 13 children with asthma who received slow release theophylline in a dosage of 15.2 mg/body weight/24 hours in average, administered 3 times a day. The efficacy was estimated by a clinical score and the serum level was determined by isotopic mass spectrometry with 15N-theophylline as internal standard. After a period of at least 2 months of therapy it was recorded the amelioration of clinical score (with 5.09 points, that represents 36.3% of the maximum initial score) and the reducing of circadian variation of peak expiratory flow from 27% to 15%. The serum level of theophylline was of 8.25 +/- 4.16 micrograms/ml at 4 hours after administration and of 5.69 +/- 2.6 micrograms/ml at 8 hours after administration of the last dose. The individual values less than 5 micrograms/ml was found in 3 of 13 children at 4 hours and in 7 of 13 children at 8 hours after the last dose. There were no patients with toxic serum levels of theophylline (> 20 micrograms/ml). The correlation between serum level of theophylline and the dosage was weak both at 4 hours (r = 0.054) and 8 hours (r = 0.229) after the last dose. At the same dose there were found high interindividual variations. These findings are arguments for the usefulness of determination of serum levels of theophylline, that together with clinical and functional parameters allowed the individualization of the dosage.

Trace analysis of triazines and organophosphorus pesticides in water.

A method for the determination of trace levels of triazines and organophosphorus pesticides in water is presented. The extraction method is based on a solid-phase extraction on C-18 bound silica SPE cartridges. A precolumn filled with Merck C-18 bound silica and home-made C-18 bound silica have been tested at a flow-rate of 3 ml/min with comparable preconcentration yields. A SIM-MS method using a (15)N labelled internal standard has been developed for the organophosphorus pesticides. Detection limits lower than 1 microg/L have been obtained. Separations have been carried out on a conventional GC column OV 17 (1 m) and a capillary column OV 17 (25 m) with a temperature program from 150 degrees C (2 min) to 300 degrees C (rate of 6 degrees C/min).

An optical spectroscopic study of borate glasses containing uranium ions.

An optical spectroscopic investigation has been performed on some borate glasses containing 1mol % UF(4), UO(2) and UO(3). The optical data confirm the presence of uranium ions in valence stages of +6, +5 and +4. The influence of the composition of the glass matrix and of the gamma-irradiation on the redox equilibrium of uranium ions was discussed.

Determination of multiply labeled serine and glycine isotopomers in human plasma by isotope dilution negative-ion chemical ionization mass spectrometry.

A gas chromatography/negative-ion chemical ionization mass spectrometry method is presented to measure the isotopic enrichment of multiple serine and glycine isotopomers. The amino acid N-heptafluorobutyryl n-propyl ester derivatives were used. The method had good analytical linearity between 10 and 800 microg mL-1 and both precision and accuracy were 5% for plasma amino acids. Sensitivity permitted analysis of 100 pg amino acid on column. The method was applied to metabolic studies of the serine to glycine interconversion in humans. (alpha-15N)serine and (1,2-13C2)glycine were given as a single intravenous bolus to six healthy male subjects. Plasma concentration of glycine and serine were determined after addition of (alpha-15N,1,2,3-13C3) serine and (alpha-15N,1,2-13C2)glycine as internal standards to 500 microL of plasma. Since glycine and serine are rapidly interconverted by hepatic serine hydroxymethyl transferase, the resultant tracer spectrum requires deconvolution of the enrichment of four isotopomers of each amino acid. Deconvolution of the ion abundance ratios to yield tracer-to-tracee ratios for each isotopomer was done using Brauman's least squares approach.

Isotope dilution mass spectrometry for procaine determination in biological samples.

A simple, rapid and sensitive method for procaine determination is described. Isotope dilution mass spectrometry with (15N)procaine as internal standard was used. The analysis was performed at 4000 resolution by selected ion monitoring with temperature programming. The sample was measured in underivatized form in the direct inlet system. The method shows good analytical parameters: linearity between 0 and 40 micrograms ml-1, good precision and accuracy. The method was applied to the in vitro pharmacokinetic study of the metabolism of procaine in liver homogenates of Wistar rats. The method is rapid, permitting about six samples to be run per hour. Sensitivity of the method permits analysis at a signal-to-noise ratio of 5:1.

Serum theophylline analysis by isotope dilution mass spectrometry.

Serum theophylline analysis was attempted using stable isotope dilution mass spectrometry. Theophylline 15N-labelled in position 7 was used as internal standard. The analysis was performed at resolution 3000 by selected ion monitoring with temperature programming. The sample was introduced in underivatized form by means of the direct inlet probe. Good linearity was obtained in the concentration range 5-40 micrograms ml-1 with relative standard deviations less than 6%. The method is simple and permits six samples to be run per hour. Sensitivity permits analysis at 0.5 micrograms ml-1 at a signal to noise ratio 4:1.

[The experience of paramedical personnel in the cardiopulmonary resuscitation of acute cardiac patients]. / Experienta cadrelor medii în resuscitarea cardiorespiratorie la bolnavi cardiaci acuti.

The cardiac stop as well as the severe despondency of the respiratory function in the recoverable patients is a major medical urgency which causes the immediate death of the patient if efficient measures of cardiorespiratory resuscitation are not correctly and rapidly taken. The authors describe in detail the measures to be taken in such situations, presenting the experience of the medical and nursing staff in the coronary intensive care unit of the Medical Clinic III, in the Clinical Hospital of Bucharest. It is underlined the fact that due to the nature of their tasks, the nursing staff have an essential contribution within the "team work" of the coronary intensive care units.