To enhance the ionization efficiencies in atmospheric pressure photoionization mass spectrometry a dopant with favorable ionization energy such as chlorobenzene is typically used. These dopants are typically toxic and difficult to mix with water-soluble organic solvents. In order to achieve a more efficient and less toxic dopant, a multicomponent mixed ...

Tissue microarrays were originally developed to enable alignment of multiple tissue cores in a single paraffin block and to enable high-throughput laboratory analysis. However, a major drawback is the loss of tissue cores during slide preparation, especially when sectioning the tissue block. Tissue cylinders directly aligned in the metal box ...

Quantitative multinuclear high-resolution magic angle spinning was performed in order to determine the tissue pH values of and the absolute metabolite concentrations in 33 samples of human brain tumour tissue. Metabolite concentrations were quantified by 1D (1)H and (31)P HRMAS using the electronic reference to in vivo concentrations (ERETIC) synthetic ...

To investigate the absorption and metabolism of 4-hydroxyderricin and xanthoangelol, we established an analytical method based on liquid chromatography-tandem mass spectrometry and measured these compounds in the plasma, urine, feces, liver, kidney, spleen, muscle and white adipose tissues of mice orally administered with Ashitaba extract (50-500mg/kg body weight). 4-Hydroxyderricin and ...

A simple and rapid method to determine the cypermethrin (CYP) insecticide in rat tissues (kidney, liver and brain) and blood has been developed for the first time using low density solvent-dispersive liquid-liquid microextraction (LDS-DLLME) followed by gas chromatography-electron capture detector (GC-ECD) analysis. Initially, tissue samples containing CYP were homoginized in ...

Flavonoid composition and concentration were investigated in 12 different tissues of 'Ti-1' lotus (Nelumbo nucifera) by high performance liquid chromatography equipped with photodiode array detection tandem electrospray ionization mass spectrometry (HPLC-DAD-ESI-MS(n)). A total of 20 flavonoids belonging to six groups (myricetin, quercetin, kaempferol, isohamnetin, diosmetin derivatives) were separated and identified. ...

Partition coefficients (PCs) are used in physiologically based pharmacokinetic (PBPK) models to estimate the free concentration of a chemical in specific blood or organs. Biological PC(tissue:blood) (tissue to blood) values were determined for a series of nonvolatile herbicides, insecticides, and fungicides in liver, brain, skin, fat, kidneys, and muscle of ...

Quantification of the physical properties of tissue biopsies and cell-remodeled hydrogels is critical for understanding tissue development and pathophysiological tissue remodeling. However, due to the low modulus, small size, irregular shape, and anisotropy of samples from these materials, accurate viscoelastic characterization using standard rheometric methods is problematic. The goal of ...

In this study we compared two polymerase chain reaction (PCR) methods using either 16S ribosomal RNA (rRNA) or 23S rRNA gene primers for the detection of different Leptospira interrogans serovars. The performance of these two methods was assessed using DNA extracted from bovine tissues previously inoculated with several bacterial suspensions. ...

Accumulation of advance glycation end products (AGEs) in vivo is associated with aging, diabetes, Alzheimer's disease, renal failure, etc. The objective of this study was to investigate the inhibitory effects of brown algae Fucus vesiculosus phlorotannins on the formation of AGEs. F. vesiculosus phlorotannins were extracted using 70% acetone. The ...

Liquid chromatography coupled to negative electrospray ionization (ESI) tandem mass spectrometry (MS/MS) employing a time-of-flight tandem mass spectrometer was used in the structural determination of phenolic compounds and sesquiterpenoids occurring in the extract from Artemisia rupestris L. A total of 91 compounds including chlorogenic acid derivatives, flavonoids (aglycone, O-glycosyl, C-glycosyl ...

The flower volatile compounds (FVCs) of two tetraploid Freesia hybrida (pink-yellow and yellow) cultivars and their cut flowers were analysed by headspace solid-phase microextraction combined with gas chromatography-mass spectrometry. Twelve FVCs were identified in the pink-yellow cultivar, with linalool as the major compound; 30 FVCs were identified in the yellow ...

Cleanup technology and mass spectrometric determination of sphingosine-1-phosphate using a -phosphate capture molecule are shown. The protocol is rapid, requires neither thin-layer chromatography nor liquid chromatography, and is applicable to both blood and solid tissue samples.

Many Drosophila tissues (other than embryos or egg chambers) are too large, delicate, transparent, or buoyant for manipulation in suspension. Tissues such as spermatocytes, spermatids, and imaginal disks are difficult to handle in suspension and are more appropriately fixed on slides or coverslips for whole-mount fluorescent in situ hybridization (FISH). ...

Direct mass spectrometric analysis of aberrant protein glycosylation is a challenge to the current analytical techniques. Except lectin affinity chromatography, no other glycosylation enrichment techniques are available for analysis of aberrant glycosylation. In this study, we developed a combined chemical and enzymatic strategy as an alternative for the mass spectrometric ...

The ability to measure steroid hormone concentrations in blood and urine specimens is central to the diagnosis and proper treatment of adrenal diseases. The traditional approach has been to assay each steroid hormone, precursor, or metabolite using individual aliquots of serum, each with a separate immunoassay. For complex diseases, such ...

A selective method has been developed for determining the concentration of 4,4'-, 3,4'-, and 2,2'-diaminodiphenylethers in sediment samples from the sea, using liquid chromatography/tandem mass spectrometry (LC/MS/MS). 4,4'-diaminodiphenylether is a suspected toxic compound, and categorized as "Class I Designated Chemical Substance" in Japan. We have investigated the levels of 4,4'-diaminodiphenylether ...

In this report, we examine the performance of a mass spectrometry (MS)-based method for quantification of protein posttranslational modifications (PTMs) using stable isotope-labeled internal standards. Uniform labeling of proteins and highly similar behavior of the labeled vs nonlabeled analyte pairs during chromatographic separation and electrospray ionization (ESI) provide the means ...

A new analytical method was developed to determine the presence of six (6) compounds with the potential to be used in economic adulteration to enhance the nitrogen content in milk products and bulk proteins. Residues were extracted from the matrix with 2% formic acid, after which acetonitrile (ACN) was added ...

In this study fifty samples of crystalline methamphetamine obtained from antinarcotics police of Iran seized during the year 2010 were analyzed. In order to determine the chemical characteristics of these samples, anion test, Gas Chromatography-Mass Spectrometry (GC-MS) and Liquid Chromatography-Mass Spectrometry (LC-MS) were carried out on the samples. All of ...

: Gamma-hydroxybutyric acid (GHB) has become one of the most dangerous illicit drugs of abuse today. It is used as a recreational and date rape drug because of its depressant effect on the central nervous system, which may cause euphoria, amnesia, respiratory arrest, and coma. There is an urgent need ...

The present methodology was developed to simultaneously assess chronic exposure to PAHs and to tobacco from the analysis of one hair specimen per examined individual. The method is a two step extraction of twelve mono-hydroxy-PAHs and of nicotine, and their separate analysis by optimized methods using gas chromatography-negative chemical ionization-mass ...

In the present work, a highly sensitive method based on solid phase microextraction and gas chromatography tandem (triple quadrupole) mass spectrometry was used to test hair samples for 50 pesticides including 39 molecules from different chemical families currently used in agriculture and 11 organochlorines. The population investigated was composed of ...

Biological activities of immunoglobulin G such as effector functions via Fc receptor interactions are influenced by Fc-linked N-glycans. Here we describe a fast, robust and sensitive nano-LC-ESI-MS method for detailed subclass specific analysis of IgG Fc N-glycosylation. A sheath-flow ESI sprayer was used as a sensitive zero dead volume plug-and-play ...

The vaporization enthalpies of (S)-ibuprofen and (S)-naproxen measured by correlation gas chromatography at T = 298.15 K are reported and compared with literature values. Adjustment of the fusion enthalpies of (RS)- and (S)-ibuprofen and (S)-naproxen to T = 298.15 K and combined with the vaporization enthalpy of the (S)-enantiomer of ...

Abstract Background: There is no certified control material for hemoglobin analysis which has the hemoglobin (Hb)A(2)/E level as high as found in ?-thalassemia trait, HbE trait, ?-thalassemia/HbE disease and homozygote of HbE, the thalassemia types found frequently in the Southeast Asian population. The aim of this study was to prepare ...

Glycosylation analysis of recombinant glycoproteins is of importance for the biopharmaceutical industry and the production of glycoprotein pharmaceuticals. A commercially available lectin array technology was evaluated for its ability to present a reproducible fingerprint of a recombinant CTLY4-IgG fusion glycoprotein expressed in large scale CHO-cell fermentation. The glycosylation prediction from ...

To establish a rapid and simple fluorescence polarization immunoassay method for determination of norvancomycin serum concentration, we collected 300 serum samples from the patients receiving norvancomycin in the hospitals localized in Shanghai, China. The drug concentrations were measured by the established HPLC method and FPIA with vancomycin kit. A FPIA ...

Thromboelastography (TEG) is a point-of-care whole blood test of hemostasis. While TEG is becoming more widely used in veterinary medicine, few studies describe the use of TEG in cats. The objectives of the current study were to: 1) document the range of TEG variables produced in healthy cats using 3 ...

A new ultrafast quantitative and high-throughput mass spectrometric method using matrix-assisted laser desorption/ionization triple quadrupole tandem mass spectrometry has been developed and validated for determination of intracellular erythrocyte concentrations of the antifolate drug methotrexate (MTX) and its polyglutamate metabolites. The method consists of a solid-phase extraction of MTX and MTX-polyglutamate ...

This article presents results from 1872 hair samples, which were analyzed for fatty acid ethyl esters (FAEEs) and ethyl glucuronide (EtG). The results were evaluated in the context of self-reported drinking behavior, the use of hair cosmetics, the gender of the sample donors and hair sample length. For comparison, CDT ...

DNA analysis is currently the easiest way to identify a hemoglobin variant in most cases. Nevertheless, in case of complex gene rearrangements, mass spectrometry studies may be required to orientate the DNA diagnosis. The present report shows the use of mass spectrometry techniques prior to DNA analysis for the identification ...

Capillary electrophoresis electrospray-mass spectrometry was used to detect and characterize the great variety of O- and N-glycopeptide glycoforms of recombinant human erythropoietin (rhEPO) using an orthogonal accelerating time-of-flight mass spectrometer to obtain their exact molecular masses (CE-TOF-MS). rhEPO was digested with trypsin and Glu-C and analyzed by CE-TOF-MS to detect ...

A simple HPLC technique for determining mitragynine, codeine, caffeine, chlorpheniramine and phenylephrine in 'kratom cocktail' was developed. The analytical method for mitragynine, codeine and caffeine used an Eclipse XDB-C8 column. A Lichrospher CN column was using for analysing chlorpheniramine and phenylephrine. The correlation coefficient of each standard was between 0.9957 ...

The development of a MALDI-TOF MS method for the quantitative analysis of the glycosylation of CHO-expressed biotherapeutic glycoproteins shall be presented. The method utilizes a well-established chemistry, reductive amination of glycans, to derivatize glycans with either a light analog ((12)C(7) anthranilic acid) or a heavy analog ((13)C(7) anthranilic acid) to ...

SUMMARYCulicoides biting midges are of great importance as vectors of pathogens and elicitors of allergy. As an alternative for the identification of these tiny insects, matrix-assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF MS) was evaluated. Protein mass fingerprints were determined for 4-5 field-caught reference (genetically confirmed) individuals of ...

The increased availability of new psychoactive substances ("legal highs") from retail shops or internet sources has caught the imagination of consumers, law enforcement and scientific communities. The present study describes the identification of 2-(diphenylmethyl)pyrrolidine (DPMP, desoxy-D2PM) as the key constituent found in an internet product called "A3A New Generation". Analytical ...

In this study, the extraction of γ-hydroxybutyrate (GHB) from urine using solid-phase extraction (SPE) is described. SPE was performed on anion exchange columns after samples of urine had been diluted with de-ionized water. After application of the diluted samples containing GHB-d(6) as an internal standard, the sorbent was washed with ...

Although DNA analysis is needed for characterization of the mutations that cause β-thalassaemia, measurement of the Hb A(2) is essential for the routine identification of people who are carriers of β-thalassaemia. The methods of quantitating Hb A(2) are described together with pitfalls in undertaking these laboratory tests with particular emphasis ...

The evaluation of glycated hemoglobin (HbA(1c)) is used in daily practice for monitoring the diabetes mellitus. HbA(1c) may be assayed by different methods, among which high-pressure liquid chromatography (HPLC). We have evaluated a new kit 2.0 available on HPLC Variant II(®) Turbo analyzer (Bio-Rad), which is characterized by an elution ...

We present herein an efficient mass spectrometric method for the localization of the glycation sites of a model neoglycoconjugate vaccine formed by a construct of the tetrasaccharide side chain of the Bacillus anthracis exosporium and the protein carrier bovine serum albumin. The glycoconjugate was digested with both trypsin and GluC ...

Haemoglobin (Hb) abnormalities though quite frequent, are generally detected in populations during surveys and programmes run for prevention of Hb disorders. Several methods are now available for detection of Hb abnormalities. In this review, the following are discussed: (i) the methods used for characterization of haemoglobin disorders; (ii) the problems ...

Background: The hemoglobincyanide method (HiCN) method for measuring hemoglobin is used extensively worldwide; its advantages are the ready availability of a stable and internationally accepted reference standard calibrator. However, its use may create a problem, as the waste disposal of large volumes of reagent containing cyanide constitutes a potential toxic ...

Glycation of IgG can result from incubation with a reducing sugar in vitro or during circulation in vivo. Upon injection of a recombinantly produced human therapeutic IgG into humans, changes in the glycation levels could be observed as a function of circulation time. Mass changes on the individual IgG polypeptide ...

A specific, sensitive and rapid analytical procedure based on capillary electrophoresis with UV/Vis detection at 405 and 415 nm was developed and validated to detect human haemoglobin and haemoglobin-based oxygen carriers (Hemopure(®) , Oxyglobin(®) and Polyheme(®) ) in blood samples collected for doping control. The electrophoretic separation, based on capillary dynamic ...

Many diseases are characterized by the changes of either glycan structure or glycosylation site of glycoproteins. The glycan profiling can provide the overview of glycosylation in despite of the absence of the glycosylation sites, which in turn simplifies the complexity of disease diagnosis. Herein, we describe a simple method to ...

Characterization of protein glycosylation requires highly specific methods for the enrichment of glycopeptides because of their sub-stoichiometric glycosylation-site occupancy. The hydrophilic affinity based strategy has attracted more attention, owing to its broad glycan specificity, good reproducibility, and compatibility with mass spectrometric (MS) analysis. Several polar matrices have emerged for hydrophilic ...

Comprehensive glycoprotein characterization based on mass spectrometry (MS) is challenging because of low concentration of glycopeptides and suppression effect of abundant non-glycosylated peptides in MS. Therefore, it is vital to enrich glycopeptides before MS analysis. A new method was developed to selectively enrich glycopeptides from complex sample by coupling C18 ...

Liquid chromatography mass spectrometry (LC-MS) peptide mapping can be a versatile technique for characterizing protein glycosylation sites without the need to remove the attached glycans as in conventional oligosaccharide mapping methods. In this way, both N-linked and O-linked sites of glycosylation can each be directly identified, characterized, and quantified by ...

Polychlorinated biphenyls (PCBs) levels were assessed in human hair samples, originating from two main agricultural regions of Greece. The analysis was performed by gas chromatography-mass spectrometry (GC-MS) and gas chromatography-double focusing high resolution mass spectrometry (GC-DFHRMS). The main analytical procedure involved hair decontamination, solid-liquid extraction and cleanup steps. The recoveries ...