Search PubMed⌕ Search

SEARCH · Search PubMed

Results for “Biological samples”

Search indexed PubMed citations on genomics, clinical trials, systematic reviews and public health. Explore titles, authors and supplied subject terms, then open the PubMed record.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 541 records · Page 30Linked to original sources
PubMed2006

A simple and sensitive analytical method for the determination of antimony in environmental and biological samples.

The results of a study and application of leucocrystal violet for the determination of antimony in parts per million levels is described here. The proposed method is based on the reaction of antimony(III) with acidified potassium iodate to liberate iodine. The liberated iodine selectively oxidizes leucocrystal violet to crystal violet dye. The formed dye shows maximum absorbance at 590 nm. The color system obeys Beer's law in the concentration range from 0.4 - 3.6 microg antimony per 25 ml of final solution. The molar absorptivity and Sandell's sensitivity were found to be 7.32 x 10(5) l mol(-1) cm(-1) and 0.0016 microg cm(-2), respectively. All variables were studied in order to optimize the reaction. The proposed method is satisfactorily applicable for the analysis of antimony in various environmental and biological samples. The method is simple, highly sensitive, accurate and reliable.

Antimony↗
PubMed2003

Morin applied in speciation of aluminium in natural waters and biological samples by reversed-phase high-performance liquid chromatography with fluorescence detection.

A reversed-phase high-performance liquid chromatographic method with fluorescence detection for the determination of labile monomeric aluminium has been developed through pre-column complexation using morin as the analytical reagent. The highly fluorescent aluminium-morin complex (excitation wavelength 418 nm, emission wavelength 490 nm) was separated on a Spherisorb ODS 2 column with an eluent consisting of 30% methanol and 70% water (pH 1.0 with perchloric acid). The most remarkable point of this protocol was that only the most toxic aluminium species, that is, free aqua-aluminium ion and its monomeric hydroxo complex ions, selectively respond among various aluminium complexes. This strategy has been successfully applied to direct fractionation of the toxic aluminium in natural waters and biological samples without any pretreatment.

Aluminum↗
PubMed1986

Alkaline hydrolysis of N-ethylmaleimide allows a rapid assay of glutathione disulfide in biological samples.

The estimation of glutathione disulfide (GSSG) is based on the NADPH-dependent glutathione reductase reaction. A new method has been developed to eliminate the inactivating effect of N-ethylmaleimide (NEM), added to prevent glutathione oxidation, on glutathione reductase. This method takes advantage of instability of NEM in alkaline solutions. The product of NEM hydrolysis, N-ethylmaleamic acid, obtained under accurate pH-controlled conditions, is compatible with a good activity of glutathione reductase which allows total recovery and measurement of GSSG. The method, applied to estimation of GSSG content in human erythrocytes and rat liver, gives results in optimum agreement with values reported in literature. Because of its simple performance and rapidity, the procedure can be considered an improved method in removing NEM and is particularly advantageous when a large number of biological samples must be treated and estimated.

Animals↗
PubMed2004

[Psychoactive substances in biological samples--toxicological laboratory data].

The subject of the research was the analysis of frequency and type of psychoactive substances used, basing on the determinations the blood and/or urine samples, performed in the toxicological laboratory of the Department of Clinical and Industrial Toxicology Jagiellonian University in Kraków in the period from December 2001 to November 2003. From 17,649 performed determinations--45.5% were positive. 50% of the positive determinations were psychoactive substances. The most often psychoactive substance determined was ethyl alcohol (52.86%), next benzodiazepines (17.41%), amphetamines (10.54%), opiates (8.05%), THC (6.87%), barbiturates (3.74%), and occasionally atropine and cocaine. There was observed a variety of mixed, simultaneously taking psychoactive substances, especially ethyl alcohol, opiates, amphetamine derivatives and cannabinoids. The analysis of the occurrence of psychoactive substances in biological samples from patients treated in different hospital departments, others hospitals and ordered by private persons also was performed. In the last two years 369 private patients ordered psychoactive substances determinations and 78 of them were positive.

Amphetamines↗
PubMed2006

Cyclopentanone thiosemicarbazone, a new complexing agent for copper determination in biological samples by adsorptive stripping voltammetry.

A selective and sensitive stripping voltammetric method for the determination of trace amounts of copper(II) with cyclopentanone thiosemicarbazone (CPTSC) is presented. The method is based on the adsorptive accumulation of the resulting copper-CPTSC complex on a hanging mercury drop electrode, followed by the stripping voltammetric measurements at the reduction current of the adsorbed complex at -0.37 V vs. Ag/AgCl. The optimal conditions for the stripping analysis of copper include pH 9.3, deposition time of 120 s, and a deposition potential of -0.1 V (vs. Ag/AgCl). The peak current is linearly proportional to the copper concentration over a range 3.14 x 10(-9) M to 1.57 x 10(-6) M with a limit of detection of 1.57 x 10(-9) M. The technique has been applied to the determination of copper in biological samples, like urine and whole blood.

Adsorption↗
PubMed1995

Application of a novel, plastic formed carbon as a precolumn packing material for the liquid chromatographic determination of acetylcholine and choline in biological samples.

A novel carbon material, plastic formed carbon (PFC), was prepared by mixing various amounts of pure graphite with an organic binder and pyrolysing the mixture to a "glassy carbon" at a modest final temperature of 1000-1400 degrees C. This preparation procedure allows more convenient and precise control of the final graphite adsorption characteristics. Various PFC materials were constructed and tested both as bulk adsorbents and as precolumn packings for the direct determination of ACh and Ch in brain tissue homogenates. The PFC precolumns prepared from 12.5-50% graphite, by mass, were capable of selectively removing interfering species while not adsorbing any of the desired quaternary amine analytes. The usually large solvent front was also dramatically reduced with these precolumns. These PFC precolumns are useful for the direct determination of ACh and Ch in brain tissue homogenates and other biological samples.

Acetylcholine↗
PubMed1996

Determination of isotopic ratios of L-leucine and L-phenylalanine and their stable isotope labeled analogues in biological samples by gas chromatography/triple-stage quadrupole mass spectrometry.

A gas chromatographic/triple-stage quadrupole mass spectrometric (GC/MS/MS) method for measuring very low levels of enrichment of [5,5,5-2H3]-L-leucine and [ring-13C6]-L-phenylalanine in plasma and lipoprotein hydrolysates is described. The amino acids were derivatized to their N-heptafluorobutyryl isobutyl ester derivatives and the isotope ratio was determined by GC/MS/MS in the negative-ion chemical ionization mode. Parent ions were the [M-HF]- ions and fragment ions used for quantification were [P-2HF-C3H7]- (leucine) and [P-HF-OC4H9]- (phenylalanine), respectively. The limit of quantification was about 10 pg of the labeled compound co-eluting with 20 ng of the endogenous compound. The calibration curves were linear in the investigated range from 0.1% to 100% of the labeled compound. In biological samples, the higher selectivity of GC/MS/MS compared with GC/MS was demonstrated.

Apolipoprotein A-I↗
PubMed2006

Zirconia-coated graphite adsorption bar micro-extraction combined with ETV-ICP-MS for the determination of trace amounts of Cd, Hg and Pb in environmental and biological samples.

In this work, a new and simple micro-extraction method termed graphite adsorption bar micro-extraction was developed, for the first time, for electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) determination of trace Cd, Hg and Pb. In this method, the graphite bar was first coated with zirconia and then inserted into the sample solution for extraction. The graphite bar enriched with the analytes was inserted directly into a graphite tube, and subsequently analyzed by ETV-ICP-MS according to an established temperature program. The experimental parameters, which had influence on the extraction and vaporization, were systematically investigated and the optimal experimental conditions were established. Under the optimized conditions, the detection limits of the method were 0.05, 0.42 and 0.06 pg/ml for Cd, Hg and Pb and the relative standard deviations (RSDs) for 11 replicates at the 0.1 ng/ml level were 7.4, 8.2 and 7.7%, respectively. The proposed method was successfully applied to the determination of trace Cd, Hg and Pb in environmental and biological samples. The results of the experiments indicate that the method has a high enrichment factor and sample utilization efficiency. Furthermore, the method is fast and environment-friendly.

Adsorption↗
PubMed1994

Analysis of malondialdehyde in biological samples by capillary gas chromatography.

An analytical method to measure malondialdehyde (MDA) was developed. MDA was derivatized with N-methylhydrazine (NMH) to 1-methylpyrazole (1-MP). 1-MP was extracted and analyzed by capillary gas chromatography with nitrogen-phosphorus detection. Analyte concentration, pH, and matrix effects of 1-MP-spiked samples were investigated to determine optimal recovery conditions. Efficiencies for solid-phase extraction ranged from 95.6 +/- 0.9 to 81.6 +/- 3.5% compared to 75.0 +/- 6.4 to 67.5 +/- 9.6% for liquid-liquid extraction for 20 to 1 nmol/ml 1-MP-spiked samples, respectively. Solid-phase extraction of 1-MP was more effective than liquid-liquid extraction over a range of pH 2-8.5 and in various aqueous matrices. Addition of methanol to the matrix decreased the solid-phase extraction efficiency. Reaction yield at pH 2-8.5 showed full conversion of MDA to 1-MP following reaction with NMH. Recovery of bound MDA was investigated by incubating bovine serum albumin (BSA) spiked with MDA at 37 degrees C for 18 h and separating the free MDA and MDA-bound protein. The recovery of bound MDA from BSA increased by increasing the acidity and temperature. Specific applications of this method for biological samples are given for the analysis of endogenous MDA in the plasma and red blood cells of mice and the formation of MDA in ultraviolet-irradiated cells in culture.

Animals↗
PubMed2002

Spectrophotometric determination of copper in pharmaceutical and biological samples with 3-[2-[2-(2-hydroxyimino-1-methyl-propylideneamino)-(ethylamino]-ethyl-imino]-butan-2-one oxime).

3-[2-[2-(2-hydroxyimino-1-methyl-propylideneamino)-ethylamino]-ethyl-imino]-butan-2-one oxime, (H(2)mdo) reacts with copper(II) to form a highly stable 1:1 complex in alkaline medium at room temperature. The complex gives a maximum absorption at 570 nm with a molar absorptivity coefficient of 0.16 x 10(4) l mol(-1) cm(-1). A spectrophotometric method using this ligand was developed and optimized in terms of pH, stability of the complex, amount of reagent required, sensitivity, linearity and tolerance limits of various foreign ions. The linear range for copper determination is 0.2-225 mg l(-1). The method is sensitive, accurate and tolerant to many foreign substances, and, all the reagents used are stable under the conditions. Moreover, the method is easy to perform for the determination of copper in pharmaceutical and biological samples.

Copper↗
PubMed1977

Analysis of drugs by pyrolysis. I. Selected ion monitoring combined with a pyrolysis method for the determination of carpronium chloride in biological samples.

In order to establish an analytical method for carpronium chloride, a parasympathomimetic agent, the pyrolysis reaction of carpronium chloride was examined in a g.c.m.s. system, which revealed that gamma-butyrolactone was produced directly from the drug as the main pyrolysis product. In the case of conversion of [2,2,3,3-2H4]carpronium chloride into the deuterated gamma-butyrolactone, 2H/1H scrambling was observed and confirmed to occur during the pyrolysis process of the deuterated compound. The proportion of gamma-[2H4]butyrolactone among the pyrolysis products was almost independent of the operating conditions, so [2,2,3,3-2H4]carpronium chloride was of practical use as an internal standard for selected ion monitoring. By incorporation of the pyrolysis reaction of carpronium chloride with selected ion monitoring and the use of [2,2,3,3-2H4]carpronium chloride as an internal standard, a rapid, sensitive and selective method was devised for the determination of the drug in biological samples. The method was utilized successfully for the biopharmaceutical studies of carpronium chloride in ma.

4-Butyrolactone↗
PubMed1990

Beta camera for static and dynamic imaging of charged-particle emitting radionuclides in biologic samples.

A detection system based on microchannel plates has been constructed to image charged particles emitted by radionuclides in biomedical samples. This technique has significant advantages over conventional film autoradiography for investigating the distribution of radiolabeled compounds: shorter acquisition times due to the high sensitivity, easier sample handling, direct quantification and the ability to perform dynamic studies. The detector performance shows a spatial resolution of 0.9 mm for carbon-14 (14C) (0.156 MeV), good linearity and homogeneity. The noise level is below 50/(cm2.sec). Successful imaging with this system has been performed with beta-emitters 14C, sulfur-35 (35S), iodine-131 (131I), yttrium-90 (90Y), and positron emitters gallium-68 (68Ga), and fluorine-18 (18F). Dynamic studies of axonal transport of 35S-methionine in a nerve, and static images of 90Y-labeled monoclonal antibodies in slices of tumors are presented. The system shows promise for rapid quantitative imaging of charged-particle emitting radionuclides in small biologic samples.

Animals↗
PubMed2006

Comparative quantification of sphingolipids and analogs in biological samples by high-performance liquid chromatography after chloroform extraction.

Sphingosine 1-phosphate (S1P) is an extra- and intracellular messenger that specifically activates five G-protein-coupled cell surface receptors designated S1P(1-5). The S1P(1) receptor is particularly important for the maintenance of immune surveillance by regulating egress of lymphocytes from thymus and secondary lymphoid organs. S1P is generated through phosphorylation of sphingosine which is catalyzed by sphingosine kinase types 1 and 2. The immunosuppressant and sphingosine analog Fingolimod (2-amino-2-(2-[4-octylphenyl]ethyl)-1,3-propanediol, FTY720) can also be phosphorylated and induces lymphopenia by downregulating cell surface expression of the S1P(1) receptor on lymphocytes. To analyze the role of S1P in lymphocyte circulation and distribution we established a high-performance-liquid-chromatography-based method for parallel detection and quantification of Fingolimod, sphingosine, and dihydrosphingosine together with their phosphorylated derivatives Fingolimod-phosphate, S1P, and dihydrosphingosine 1-phosphate. Phosphorylated and nonphosphorylated lipids were efficiently isolated from biological samples such as cells, tissues, serum, plasma, and media by simple chloroform extraction. Fluorescence labeling with 9-fluorenylmethyl chloroformiate ensured high selectivity and enhanced sensitivity for sphingolipid detection. The described method provides an accurate approach to investigate phosphorylation, dephosphorylation, hydrolyzation, and dehydrolyzation of sphingolipids and analogs. In addition it works independently from enzymatic conversions, measuring actual concentrations rather than enzymatic activities.

Animals↗
PubMed2000

Determination of nicotine N-1-glucuronide, a quaternary N-glucuronide conjugate, in human biological samples.

[Methyl-d3]-N-1-beta-D-glucopyranosyl-(+/-)-nicotinium inner salt ((+/-)-[methyl-d3]nicotine N-1-glucuronide) was synthesized from (+/-)-[methyl-d3]nicotine via reaction with methyl-2,3,4-tri-O-acetyl-1-bromodeoxy-alpha-D-glucopyranouronate, followed by deprotection with 1 M aqueous NaOH and purification by preparative TLC. Nicotine N-glucuronide was identified and determined directly in smokers' urine. A solid phase extraction method was used to partially isolate the material from urine. Subsequent determination was by thermospray-LC/MS using the synthetic d3-labeled nicotine N-glucuronide as internal standard. The identified urinary component had the same retention time as a synthetic standard and gave the same mass spectrum. The thermospray mass spectrum was characterized from the protonated molecular ion (m/z 339) and the protonated aglycone ion (m/z 163). Quantitative results from this direct method were compared with those from an indirect method, which calculated the nicotine glucuronide in the biological sample from the amount of nicotine released following treatment of the sample with the deconjugating enzyme, beta-glucuronidase. On average, the concentration of nicotine N-glucuronide determined by the direct method was 34% greater than that determined by the indirect method. Concentrations of nicotine N-glucuronide in urine ranged from 2.2 to 7.6 nmol/ml with a limit of detection of 1.3 nmol/ml.

Adult↗
PubMed1995

Orthogonal array design as a chemometric method for the optimization of analytical procedures. Part 5. Three-level design and its application in microwave dissolution of biological samples.

The theory and methodology of a three-level orthogonal array design as a chemometric method for the optimization of analytical procedures were developed. In the theoretical section, firstly, the matrix of a three-level orthogonal array design is described and orthogonality is proved by a quadratic regression model. Next, the assignment of experiments in a three-level orthogonal array design and the use of the triangular table associated with the corresponding orthogonal array matrix are illustrated, followed by the data analysis strategy, in which significance of the different factor effects is quantitatively evaluated by the analysis of variance (ANOVA) technique and the percentage contribution method. Then, a quadratic regression equation representing the response surface is established to estimate each factor that has a significant influence. Finally, on the basis of the quadratic regression equation established, the derivative algorithm is used to find the optimum value for each variable considered. In the application section, microwave dissolution for the determination of selenium in biological samples by hydride generation atomic absorption spectrometry is employed, as a practical example, to demonstrate the application of the proposed three-level orthogonal array design in analytical chemistry.

Chemistry Techniques, Analytical↗
PubMed2006

Sensitive determination of 4-(4-chlorophenyl)-4-hydroxypiperidine, a metabolite of haloperidol, in a rat biological sample by HPLC with fluorescence detection after pre-column derivatization using 4-fluoro-7-nitro-2,1,3-benzoxadiazole.

4-(4-Chlorophenyl)-4-hydroxypiperidine (CPHP), one of the metabolites of haloperidol, is considered to exhibit brain toxicity. CPHP concentrations in plasma and tissue homogenates (each 200 microL) from rats were analyzed by HPLC fluorescence detection after pre-column derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F). After basic extraction of the samples with benzene, the derivatization with NBD-F was conducted in borate buffer (pH 8.0) at 60 degrees C for 3 min. Mexiletine was carried through the procedure as an internal standard. The regression equation for CPHP showed a good linearity in the range of 0.03-1 microg/mL with a detection limit of 0.008 microg/mL. The coefficient of variation was less than 11.6%. Plasma concentration-time courses of CPHP after intraperitoneal or per oral administration of CPHP, haloperidol or reduced haloperidol were examined, and the pharmacokinetic parameters were estimated. Additionally, CPHP levels in various tissues at 8 h after intraperitoneal administration of these compounds were compared. The method was simple and sensitive, useful for determination of CPHP in rat biological samples using as little as 200 microL of sample volume and could be applied for pharmacokinetic study.

4-Chloro-7-nitrobenzofurazan↗
PubMedDate not supplied

Screening of basic drugs in biological samples using dual column capillary chromatography and nitrogen-phosphorus detectors.

A method is presented for the extraction and screening of basic and neutral drugs, including amphetamines. Two milliliters of blood are buffered to pH 9.0 and extracted with n-chlorobutane. Underivatized extracts are analyzed simultaneously on two complementary capillary columns placed together in one injection port using split injection. A relative retention time list comprised of 110 common drugs of abuse and metabolites has been compiled for both capillary columns. The internal standard used is SKF-525A. The success of the method depends upon four areas: inertness of the system, nitrogen detector optimization, extraction technique, and lack of contamination. The percent recovery has been calculated for twelve commonly encountered drugs. The within-run and day-to-day recoveries and retention time reproducibility have been investigated for the internal standard SKF-525A. The authors have found the combination of fused silica capillary columns and nitrogen-phosphorus detectors makes for a stable screening system for basic and neutral drugs in biological samples.

Chromatography↗
PubMedDate not supplied

Quantification and significance of protein oxidation in biological samples.

Protein oxidation is defined here as the covalent modification of a protein induced either directly by reactive oxygen species or indirectly by reaction with secondary by-products of oxidative stress. Oxidative modification of proteins can be induced experimentally by a wide array of prooxidant agents and occurs in vivo during aging and in certain disease conditions. Oxidative changes to proteins can lead to diverse functional consequences, such as inhibition of enzymatic and binding activities, increased susceptibility to aggregation and proteolysis, increased or decreased uptake by cells, and altered immunogenicity. There are numerous types of protein oxidative modification and these can be measured with a variety of methods. Protein oxidation serves as a useful marker for assessing oxidative stress in vivo. There are both advantages and disadvantages to using proteins for this purpose compared to lipids and DNA. Finally, it is important to monitor the degree of oxidative modification of therapeutic proteins manufactured for commercial use. This review will examine various aspects of protein oxidation, with emphasis on using proteins as markers of oxidative stress in biological samples.

Biomarkers↗