scholarly journals Perfluorinated compounds in red-throated divers from the German Baltic Sea: new findings from their distribution in 10 different tissues

2011 ◽  
Vol 8 (4) ◽  
pp. 419 ◽  
Author(s):  
Janne Rubarth ◽  
Annekatrin Dreyer ◽  
Nils Guse ◽  
Jürgen W. Einax ◽  
Ralf Ebinghaus
Keyword(s):  
Baltic Sea ◽  
High Performance ◽  
Body Burden ◽  
Standard Addition ◽  
Perfluorinated Compounds ◽  
Fatty Tissue ◽  
Environmental Matrices ◽  
Multivariate Statistical ◽  
Tissue Samples ◽  
New Findings

Environmental contextPerfluorinated compounds are commonly used chemicals that are detected globally in all environmental matrices. We investigated the extent of contamination by perfluorinated compounds in the red-throated diver, a marine predatory bird, and observed an unusual distribution of perfluorinated compounds in tissues. The data help us to better understand the behaviour of these contaminants in organisms. AbstractTwenty poly- and perfluorinated compounds (PFCs) were investigated in four red-throated divers (Gavia stellata) from the German Baltic Sea sampled in 2005. Concentrations of perfluoroalkyl sulfonates (PFSAs), perfluoroalkyl carboxylates (PFCAs), alkylated perfluoroalkyl sulfonamides, alkylated perfluoroalkyl sulfonamidoethanols and perfluorooctane sulfonamides were determined in blood, brain, fatty tissue, gall bladder, heart, kidney, liver, lung, muscle and spleen by high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). For quantification standard addition was applied. Twelve compounds were detected with average total PFC concentrations ranging from 42 ng g–1 in muscle to 220 ng g–1 in liver samples. Perfluorooctane sulfonate (PFOS) was the major compound in each of the 40 tissue samples. Except for brain, perfluoroundecanoate was the dominant PFCA. In brain samples preferential enrichment of long-chain PFSAs and PFCAs was observed. The total PFC body burden was estimated to 100 ± 39 µg. Multivariate statistical analyses supported the identification of the preferred accumulation ‘location’ of individual PFCs in the birds’ body.

scholarly journals Preparative, extraction, and analytical methods for simultaneous determination of legacy and insensitive munition (IM) constituents in aqueous, soil or sediment, and tissue matrices

2021 ◽  
Author(s):  
Rebecca Crouch ◽  
Jared Smith ◽  
Bobbi Stromer ◽  
Christian Hubley ◽  
Samuel Beal ◽  
...  
Keyword(s):  
High Performance ◽  
Solid Phase ◽  
Direct Injection ◽  
Treatment Method ◽  
Extraction Methods ◽  
Environmental Matrices ◽  
Long Term Effects ◽  
Tissue Samples ◽  
New Methods ◽  
Supply Costs

No standard method exists for determining levels of insensitive munition (IM) compounds in environmental matrices. This project resulted in new methods of extraction, analytical separation and quantitation of 17 legacy and 7 IM compounds, daughter products of IM, and other munition compounds absent from USEPA Method 8330B. Extraction methods were developed for aqueous (direct-injection and solid-phase extraction [SPE]), soil, sediment, and tissue samples using laboratory-spiked samples. Aqueous methods were tested on 5 water sources, with 23 of 24 compounds recovered within DoD QSM Ver5.2 limits. New solvent extraction (SE) methods enabled recovery of all 24 compounds from 6 soils within QSM limits, and a majority of the 24 compounds were recovered at acceptable levels from 4 tissues types. A modified chromatographic treatment method removed analytical interferences from tissue extracts. Two orthogonal high-performance liquid chromatography-ultraviolet (HPLC-UV) separation methods, along with an HPLC–mass spectrometric (HPLC-MS) method, were developed. Implementing these new methods should reduce labor and supply costs by approximately 50%, requiring a single extraction and sample preparation, and 2 analyses rather than 4. These new methods will support environmental monitoring of IM and facilitate execution of risk-related studies to determine long-term effects of IM compounds.

scholarly journals Multi-Spheres Adsorptive Microextraction (MSAμE)—Application of a Novel Analytical Approach for Monitoring Chemical Anthropogenic Markers in Environmental Water Matrices

Molecules ◽  
2019 ◽  
Vol 24 (5) ◽  
pp. 931 ◽  
Author(s):  
Ana Silva ◽  
Nuno Neng ◽  
José Nogueira
Keyword(s):  
High Performance ◽  
Activated Carbons ◽  
Standard Addition ◽  
Environmental Water ◽  
Environmental Matrices ◽  
Experimental Conditions ◽  
Anthropogenic Markers ◽  
Feasible Alternative ◽  
Environmental Water Matrices ◽  
Wastewater Samples

Multi-spheres adsorptive microextraction using powdered activated carbons (ACs) was studied as a novel enrichment approach, followed by liquid desorption and high-performance liquid chromatography with diode array detection (MSAµE(AC)-LD/HPLC-DAD) to monitor caffeine (CAF) and acetaminophen (ACF) traces in environmental matrices. In this study, commercial activated carbons (N, NOX, and R) were tested, with the latter showing a much better performance for the analysis of both anthropogenic drugs. The main parameters affecting the efficiency of the proposed methodology are fully discussed using commercial AC(R). Textural and surface chemistry properties of the ACs sample were correlated with the analytical results. Assays performed on 30 mL of water samples spiked at 10 µg L−1 under optimized experimental conditions, yielding recoveries of 75.3% for ACF and 82.6% for CAF. The methodology also showed excellent linear dynamic ranges for both drugs with determination coefficients higher than 0.9976, limits of detection and quantification of 0.8–1.2 µg L−1 and 2.8–4.0 µg L−1, respectively, and suitable precision (RSD < 13.8%). By using the standard addition method, the application of the present method to environmental matrices, including superficial, sea, and wastewater samples, allowed very good performance at the trace level. The proposed methodology proved to be a feasible alternative for polar compound analysis, showing to be easy to implement, reliable, and sensitive, with the possibility to reuse and store the analytical devices loaded with the target compounds for later analysis.

scholarly journals Comparative Research of Chemical Profiling in Different Parts of Fissistigma oldhamii by Ultra-High-Performance Liquid Chromatography Coupled with Hybrid Quadrupole-Orbitrap Mass Spectrometry

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 960
Author(s):  
Haibo Hu ◽  
Yau Lee-Fong ◽  
Jinnian Peng ◽  
Bin Hu ◽  
Jialin Li ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
High Resolution Mass Spectrometry ◽  
Scientific Development ◽  
Multivariate Statistical ◽  
Accurate Identification ◽  
Orbitrap Mass Spectrometry ◽  
Q Exactive

The roots of Fissistigma oldhamii (FO) are widely used as medicine with the effect of dispelling wind and dampness, promoting blood circulation and relieving pains, and its fruits are considered delicious. However, Hakka people always utilize its above-ground parts as a famous folk medicine, Xiangteng, with significant differences from literatures. Studies of chemical composition showed there were multiple aristolactams that possessed high nephrotoxicity, pending evaluation research about their distribution in FO. In this study, a sensitive, selective, rapid and reliable method was established to comparatively perform qualitative and semi-quantitative analysis of the constituents in roots, stems, leaves, fruits and insect galls, using an Ultra-High-Performance Liquid Chromatography coupled with Hybrid Quadrupole Orbitrap Mass Spectrometry (UPLC-Q-Exactive Orbitrap MS, or Q-Exactive for short). To make more accurate identification and comparison of FO chemicals, all MS data were aligned and screened by XCMS, then their structures were elucidated according to MSn ion fragments between the detected and standards, published ones or these generated by MS fragmenter. A total of 79 compounds were identified, including 33 alkaloids, 29 flavonoids, 11 phenylpropanoids, etc. There were 54 common components in all five parts, while another 25 components were just detected in some parts. Six toxic aristolactams were detected in this experiment, including aristolactam AII, AIIIa, BII, BIII, FI and FII, of which the relative contents in above-ground stems were much higher than roots. Meanwhile, multivariate statistical analysis was performed and showed significant differences both in type and content of the ingredients within all FO parts. The results implied that above-ground FO parts should be carefully valued for oral administration and eating fruits. This study demonstrated that the high-resolution mass spectrometry coupled with multivariate statistical methods was a powerful tool in compound analysis of complicated herbal extracts, and the results provide the basis for its further application, scientific development of quality standard and utilization.

Interpretation of melperone intoxication: post-mortem concentration distribution and interpretation of intoxication data

2021 ◽  
Vol 36 (3) ◽  
pp. 233-237
Author(s):  
Marek Dziadosz ◽  
Katarina Bolte ◽  
Wolfgang Rosenberger ◽  
Michael Klintschar ◽  
Jörg Teske
Keyword(s):  
Concentration Distribution ◽  
Method Development ◽  
Standard Addition ◽  
Lethal Concentration ◽  
Post Mortem ◽  
Tissue Samples ◽  
Expert Opinions ◽  
Lack Of Information ◽  
Reference Concentration ◽  
Femoral Blood

Abstract Objectives Since melperone abuse with lethal intoxication is common, expert opinions based on therapeutical and lethal concentration ranges can be considered as important. Because there is a lack of information about fatalities caused by melperone mono-intoxications and data on tissue samples with concentration distribution, the aim of this work is the examination of lethal concentration ranges of melperone and drug quantification in different matrices. Methods An LC-MS/MS method was applied for analyses performed in blood and tissue samples. Quantification based on standard addition and sample preparation on liquid–liquid extraction with 1-chlorobutane. An appropriate tissue homogenization was performed ahead of extraction with an IKA Ultra-Turrax-Tube-Drive®. A Luna 5 µm C18 (2) 100 Å, 150  × 2 mm analytical column was used for chromatographic separation and the elution was performed with two mobile phases consisted of A (H2O/methanol = 95/5, v/v) and B (H2O/methanol = 3/97, v/v) both with 10 mM ammonium acetate and 0.1% acetic acid. Results A multi-drug LC-MS/MS analytical method developed was applied successfully for melperone quantification in different post-mortem matrices. No analytical problems could be identified during method development and analyses of real samples. The melperone lethal concentration calculated in femoral blood of the drug mono-intoxication investigated was 10 mg/L. Melperone concentration distribution was presented for the first time. Conclusions The lethal reference concentration of melperone in femoral blood of 17.1 mg/L pointed out in different reference lists should be used with caution. Instead, a lower lethal melperone concentration should be considered. The post-mortem concentration distribution of the drug presented could be helpful in the interpretation of cases where no blood samples are available.

scholarly journals Prophylactic impact of nano-selenium on performance, carcasses quality, and tissues' selenium concentration using reversed-phase high-performance liquid chromatography during microbial challenge in broiler chickens

2020 ◽  
Vol 13 (9) ◽  
pp. 1780-1797
Author(s):  
Essam S. Soliman ◽  
Fadwa F. Mahmoud ◽  
Mai A. Fadel ◽  
Rania T. Hamad
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Meat Quality ◽  
High Performance ◽  
Bacterial Load ◽  
Reversed Phase ◽  
Bursa Of Fabricius ◽  
Health Concern ◽  
Tissue Architecture ◽  
Tissue Samples

Background and Aim: Nano-selenium (NS) supplementation contributes in improving productivity, performance, and meat quality while reducing public health concern. Influence of NS and inorganic selenium (Se) water additive on performance, carcass quality, immunoglobulin concentration, intestinal microbiota, Se tissue concentrations, and tissue architecture was studied. Materials and Methods: Two-hundred and sixty 1-day-old Hubbard chicks were randomly grouped into five groups (5×52) and supplemented with 0.5 and 1.0 mL of NS and inorganic Se (100 mg.L-1). G1, G2, G3, and G4 were challenged with Escherichia coli O157: H7 2.6×108 on the 14th day. A total of 2250 samples, including 250 sera, 250 intestinal swabs, and 1500 organ and tissue samples as liver, spleen, heart, bursa, intestine, and breast muscles, and 250 eviscerated carcasses were collected. Results: The results revealed a highly significant increase (p<0.01) in live body weights, weight gains, performance indices, carcasses, and organs weights, whereas immunoglobulin G and M concentrations in broilers treated with 0.5 and 1.0 mL NS, respectively, synchronized reveal a highly significant decline (p<0.01) in total bacterial and Enterobacteriaceae counts of intestinal swabs and breast muscles, final pH24, and drip loss in broilers treated with 0.5 and 1.0 mL NS, respectively. Meanwhile, water holding capacity revealed no significant differences between all groups. Reversed-phase high-performance liquid chromatography examination revealed the earlier disappearance of NS residues than inorganic Se from the broiler's liver and muscles. Histopathological photomicrographs of the liver, spleen, bursa of Fabricius, and intestine, as well as, the immunohistochemistry of intestinal sections revealed superior tissue architecture in broilers treated with NS contrary to inorganic Se. Conclusion: The study showed significant stimulation actions of NS on performance, immunity, carcass and meat quality, intestinal and muscles' bacterial load as well as short withdrawal period and nearly normal cellular architecture compared to inorganic Se.

scholarly journals Identification of Urine Metabolic Biomarkers for Vogt-Koyanagi-Harada Disease

2021 ◽  
Vol 9 ◽  
Author(s):  
Rui Chang ◽  
Ying Zhu ◽  
Jing Xu ◽  
Lin Chen ◽  
Guannan Su ◽  
...  
Keyword(s):  
High Performance ◽  
Area Under The Curve ◽  
Enrichment Analysis ◽  
Pathway Enrichment Analysis ◽  
Healthy Controls ◽  
Roc Curve Analysis ◽  
Multivariate Statistical ◽  
Flight Mass Spectrometry ◽  
Laboratory Biomarkers ◽  
Vkh Disease

The diagnosis of Vogt-Koyanagi-Harada (VKH) disease is mainly based on a complex clinical manifestation while it lacks objective laboratory biomarkers. To explore the potential molecular biomarkers for diagnosis and disease activity in VKH, we performed an untargeted urine metabolomics analysis by ultra-high-performance liquid chromatography equipped with quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF/MS). Through univariate and multivariate statistical analysis, we found 9 differential metabolites when comparing VKH patients with healthy controls, and 26 differential metabolites were identified when comparing active VKH patients with inactive VKH patients. Pathway enrichment analysis showed that glycine, serine and threonine metabolism, and arginine and proline metabolism were significantly altered in VKH versus healthy controls. Lysine degradation and biotin metabolism pathways were significantly altered in active VKH versus inactive VKH. Furthermore, the receiver operating characteristic (ROC) curve analysis revealed that the combination of acetylglycine and gamma-glutamylalanine could differentiate VKH from healthy controls with an area under the curve (AUC) of 0.808. A combination of ureidopropionic acid and 5′-phosphoribosyl-5-amino-4-imidazolecarboxamide (AICAR) had an excellent AUC of 0.958 for distinguishing active VKH from inactive VKH. In summary, this study identified abnormal metabolites in urine of patients with VKH disease. Further studies are needed to confirm whether these metabolites are specific for this disease.

Catecholamine measurements by high-performance liquid chromatography

1984 ◽  
Vol 247 (1) ◽  
pp. E13-E20 ◽  
Author(s):  
P. Hjemdahl
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Cation Exchange ◽  
High Performance ◽  
Reversed Phase ◽  
Exchange Chromatography ◽  
Lower Sensitivity ◽  
Tissue Samples ◽  
Basal Plasma ◽  
Postcolumn Derivatization

The development of sensitive detectors has allowed the use of high-performance liquid chromatography (HPLC) for measurements of catecholamines in extracts of plasma, urine, and tissue samples. Separation of the catecholamines may be effected by reversed phase chromatography or cation-exchange chromatography and quantitation by electrochemical detection (EC) or by fluorometry coupled with postcolumn derivatization according to the trihydroxyindole (THI) method. EC has a somewhat lower sensitivity than the THI method for norepinephrine (NE) and epinephrine (E). The THI method is insensitive to dopamine (DA). Basal plasma E levels of 0.1 nM (20 pg/ml) or less may be measured in sample volumes of 1-2 ml with EC. Sensitivity and reproducibility of an assay is not necessarily a guarantee of accuracy. It is argued that new methods and modifications of old methods should be validated against accepted methodology. This is rarely the case. Cation exchange HPLC with EC has been adequately validated, but only one of the reversed phase methods has been compared with radioenzymatic methodology. HPLC has the advantages of economy, speed, and more stimulating laboratory work, as compared with radioenzymatic methodology.

scholarly journals Sensitive analysis of ethanolamine- and serine-containing phosphoglycerides by high-performance liquid chromatography

1975 ◽  
Vol 145 (3) ◽  
pp. 517-526 ◽  
Author(s):  
F B Jungalwala ◽  
R J Turel ◽  
J E Evans ◽  
R H McCluer
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Amino Groups ◽  
Tissue Samples ◽  
Primary Amino ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

A highly sensitive method for the separation and quantitative measurement of phospholipids containing primary amino groups, such as phosphatidylethanolamine, phosphatidylserine and lysophosphatidylethanolamine, is described. The method involves a simple and quantitative derivative formation of the phospholipids containing amino groups to their u.v.-absorbing biphenylcarbonyl derivatives. These have molar extinction coefficients of about 23,000 at 268nm. The phospholipid derivatives are then separated and non-destructively determined by high-performance liquid chromatography. The amino phospholipids containing vinyl ether bonds (plasmalogens) can be determined separately from the diacyl- and alkylacyl-amino phospholipids. The lower limit of detection by high-performance liquid-chromatographic analysis of the phospholipid derivatives is about 10-13pmol or 0.3-0.4ng of phospholipid P. The quantitative range of derivative formation and analysis by high-performance liquid chromatography of the phospholipids containing amino groups was shown to be 10-500nmol. The method was shown to be applicable to the analysis of phospholipids containing amino groups in tissue samples.

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