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The Analyst.
Publisher:
Chemical Society. Cambridge : Royal Society of Chemistry
Frequency: Twenty four no. a year, 2011-
Country: England
Language: English
Author(s):
Royal Society of Chemistry (Great Britain), Society for Analytical Chemistry., Society of Public Analysts (Great Britain), Society of Public Analysts and Other Analytical Chemists (Great Britain)
Start Year:1876 -
ISSN:
0003-2654 (Print)
1364-5528 (Electronic)
0003-2654 (Linking)
1364-5528 (Electronic)
0003-2654 (Linking)
Impact Factor
4.2
2022
| NLM ID: | 0372652 |
| (DNLM): | A29805000(s) |
| (OCoLC): | 01481074 |
| Coden: | ANALAO |
| Classification: | W1 AN191 |
Screening analysis of doping agents in horse urine and plasma with dilute and shoot using liquid chromatography high resolution mass spectrometry. Various technical methodologies are required to accurately detect substances of different chemical and pharmacological properties in biological samples, which are increasing in number and variety daily. Therefore, laboratories where many samples and different factors are analyzed simultaneously need methods with easy sample preparation, short analysis times and low analysis costs. In this study, the objective was to scan substances susceptible to chemical degradation, amenable to analysis without hydrolysis, and exhibiting short-term stability by employing a straightforward, expeditious, and c...
Spatially offset Raman spectroscopy for photon migration studies in bones with different mineralization levels. The ability of Spatially Offset Raman Spectroscopy (SORS) to obtain chemically specific information from below the sample surface makes it a promising technique for non-invasive in vivo diagnosis of bone conditions by sampling bone through the skin. The depth below a surface interrogated by SORS depends on the system's optical properties and is difficult to estimate for complex bone material. This paper uses 830 nm laser excitation to investigate the influence of bone mineralization on photon migration properties in deer antler cortex, equine metacarpal cortex and whale tympanic bulla. Thin sl...
A new analytical method based on anti-EPO monolith column and LC-FAIMS-MS/MS for the detection of rHuEPOs in horse plasma and urine samples. Recombinant human erythropoietin (rHuEPO) is a 30-34 kDa glycoprotein banned by the racing authorities. For some years this molecule has been detected in race horses in USA and in Europe, and even in racing camels. Although direct methods to differentiate horse endogenous EPO and rHuEPO have been developed either by LC-MS/MS or by isoelectric focusing (IEF) with double-blotting, the short confirmation time of such prohibited hormone in plasma remains a problem for horseracing doping control laboratories. In order to improve the rHuEPOs confirmation process in horse plasma or urine in terms of ...
Rapid separation and identification of the subtypes of swine and equine influenza A viruses by electromigration techniques with UV and fluorometric detection. Influenza A is viral disease, which is a cause of yearly epidemics and, potentially, pandemics. The conventional techniques used today are equipment-demanding, time-consuming and laborious. Recently, we have confirmed that the capillary isoelectric focusing is a suitable fast alternative for the verifying of virus purity. In the wide pH gradient of pH range 2.0-7.5 the isoelectric points for subtypes of equine (H3N8) and swine (H1N2) influenza A viruses were determined approximately as 6.6 and 6.5, respectively. In this contribution we have verified these findings using different isolates of d...
Detection of secondary biomarker of met-eGH as a strategy to screen for somatotropin misuse in horseracing. Since the Australian commercialisation of the recombinant equine growth hormone (reGH) in 1998 (EquiGen-5), Bresagen), this reGH, which differs only from eGH by an additional methionine at the N-terminal end (met-eGH), is worldwide suspected to be administered to racehorses as a doping agent. Indeed, the use of this biological drug is considered as a threat to horseracing since it acts both on growth, development or reproductive functions, and on the improvement of performances. In this work, we describe two reliable techniques based on surface plasmon resonance biosensor immunoassay (SPR-BIA)...
Detection of diazepam in horse hair samples by mass spectrometric methods. A method for the detection of diazepam in horse hair samples by low resolution gas chromatography-mass spectrometry (GC-MS) was developed. Two other techniques, gas chromatography-high-resolution mass spectrometry (GC-HRMS) and high-performance liquid chromatography-atmospheric pressure chemical-ionisation mass spectrometry (HPLC-APCI-MS-MS) were applied on some selected samples. Sample preparation was performed according to a technique previously described for human hair, involving incubation with Sorensen buffer and solvent extraction. Hair samples from different sites such as coat on the ne...
Determination of testosterone:epitestosterone ratio after pentafluorophenyldimethylsilyl-trimethylsilyl derivatisation using gas chromatography-mass spectrometry in equine urine. A highly specific method is described for measuring the testosterone:epitestosterone ratio in equine urine by gas chromatography-mass spectrometry (GC-MS) with stable isotope internal standards. The procedure was based on Serdolit Pad-1 resin extraction, enzymatic hydrolysis, and chemical derivatisation prior to instrumental analysis. The mixed derivatives, 3-trimethylsilyl-17-pentafluorophenyldimethylsilyl ether (3-TMS-17-flophemesyl) testosterone and epitestosterone, were found to have excellent analytical properties. The specificity of the derivatisation method exploits a unique feature of ...
Different approaches to the identification of a cortisol isomer compound in horse urine. A threshold concentration for cortisol in equine urine was fixed at 1.0 microgram ml-1 by the racing authorities in 1994. In some circumstances, interlaboratory discrepancies were observed and structural cortisol modification was revealed. In order to elucidate the degradation process and to prevent it, an identification study of the produced compound was carried out. The modified substrate was characterised by the same molecular weight as cortisol and a shorter retention time under the conditions used for the cortisol quantification (M.A. Popot, PhD Thesis, King's College, London, 1996). To i...
Nortestosterone: endogenous in urine of goats, sheep and mares? For a number of species it is known that nortestosterone, either the alpha- or beta-epimer, can be of endogenous origin. For goats and mares similar results have not yet been published. As a follow-up on the experiments with cattle, a large number of urine samples per animal were collected from pregnant goats, sheep and mares. These samples were analysed for the presence of alpha- and beta-nortestosterone and alpha-estradiol using GC-MS. The results show that in the goats and mares studied alpha-nortestosterone is present during pregnancy. In this study no alpha-nortestosterone could be demons...
Detection of quinine and its metabolites in horse urine by gas chromatography-mass spectrometry. After oral administration of quinine sulfate to a thoroughbred mare, seven urine samples were obtained over a 45.5 h period. Using gas chromatography -electron impact ionization and positive-ion chemical ionization mass spectrometry, quinine and five putative metabolites were detected and tentatively identified in enzyme-hydrolysed post-administration urine; all metabolites involved some form of oxidation. The parent drug could be detected for about 16 h and some phase I biotransformation products for up to 40 h post-administration.
Establishing the cut-off concentration for the detection of etorphine in horse urine. An 125I radioimmunoassay to determine the pattern of urinary excretion of etorphine (a semisynthetic opiate agonist) after its administration to horses is described. Three thoroughbred horses were each given 5, 15, 30 and 100 micrograms of etorphine intramuscularly. Urine was collected for up to 72 after administration. The maximum etorphine concentration after administration of a dose of 5 micrograms was 711 pg ml-1 (concentrations were greater than 100 pg ml-1 after 23 h in all three horses); a 15 micrograms gave 2661 pg ml-1 (levels remained above 100 pg ml-1 for more than 44 h in each hors...
Comparison of time-resolved fluoroimmunoassay and immunoenzymometric assay for clenbuterol. A time-resolved fluoroimmunoassay (TR-FIA) for the direct determination of clenbuterol residues in horse urine using a highly specific monoclonal antibody has been compared with an immunoenzymometric assay (IEMA). The sensitivity of both methods was 10 pg; the calibration curve was linear between 10 and 10(5) pg for the TR-FIA and between 10 and 10(4) pg for the IEMA.
Preliminary study of the metabolism of 17 alpha-methyltestosterone in horses utilizing gas chromatography-mass spectrometric techniques. Little is known about the metabolism of 17 alpha-alkyl anabolic steroids in horses. In this study, the metabolism of 17 alpha-methyltestosterone is investigated by oral administration of a (1 + 1) mixture of the steroid and its deuteriated analogue. Both compounds were synthesized from dehydroisoandrosterone (DHA), using a Grignard reaction followed by an Oppenauer oxidation. Post-administration urine extracts were analysed by gas chromatography--mass spectrometry (GC-MS) using both electron impact (IE) and chemical ionization (CI). Interpretation of the data was facilitated by observation of ...
Determination of xanthines by high-performance liquid chromatography and thin-layer chromatography in horse urine after ingestion of Guaraná powder. The seeds of Guaraná are rich in xanthines and are used for the preparation of guaraná powder which is very commonly given to horses as a 'tonic' in Brazil. In this paper, the xanthine content of guaraná powder was determined, in addition to its clearance time in horses. Thin-layer chromatography was used as a screening procedure and high-performance liquid chromatography was performed to quantify the drugs in both the powder and urine samples. The guaraná powder was found to contain 2.16, 1.10 and 36.78 mg g-1 of theobromine (TB), theophylline (TP) and caffeine (CF), respectively, and in ...
Generic immunoassay of corticosteroids with minimum pre-treatment of urine samples. A generic, rapid and sensitive enzyme linked immunosorbent assay (ELISA) test has been developed which allows large-scale simultaneous testing of synthetic corticosteroids viz., flumethasone, dexamethasone and betamethasone. This assay can be directly applied to diluted urine samples (1 + 9) without hydrolysis of glucuronide or sulfate conjugates or any other treatment of samples. The polyclonal antibody was obtained by immunizing sheep with a flumethasone derivative linked to human serum albumin. This polyclonal antibody displayed high-reactivity with several synthetic corticosteroids whilst ...
Determination of succinonitrile in horse urine by gas chromatography-nitrogen-phosphorus detector and gas chromatography-mass spectrometry. A chromatographic method was developed to detect and confirm the presence of succinonitrile (SDN) in horse urine samples, for antidoping control. The urine samples (5 ml) were extracted with diethyl ether and screened by gas chromatography-nitrogen-phosphorus detector and the confirmation of the drug's presence was accomplished by using gas chromatography-mass selective detection. The recovery of extraction was 78 and 81% for 1.0 and 2.0 micrograms ml-1 (relative standard deviation, < 10%), respectively. Urine samples collected after the administration of Energisan were positive for SDN (1-30 ...
Screening of non-steroidal anti-inflammatory drugs, barbiturates and methyl xanthines in equine urine by gas chromatography-mass spectrometry. A gas chromatographic-mass spectrometric (GC-MS) screening procedure for 23 acidic drugs in equine urine is described. With the GC-MS method fifteen anti-inflammatory drugs, five barbiturates and three methyl xanthines can be detected with good sensitivity and selectivity. The method consists of alkaline hydrolysis, extraction with organic solvent using salting-out, clean-up extraction, methylation and screening with GC-MS in selected-ion monitoring mode. The limit of detection is 10 micrograms 1(-1) or lower, for most drugs.
Endogenic nortestosterone in cattle? When residues of nortestosterone (NT) were found in the urine of cattle, racehorses or bodybuilders, exogenic administration was thought to be proven. In previous literature, no records were found of the endogenic presence of this molecule. In the horse-racing world, Houghton and Courthot found that NT is normally present in the urine of the stallion. Belgian and Dutch researchers found that NT is also present in the urine and edible parts of the intact boar. Vandenbroeck et al. (1991) suggested the endogenous presence of NT (in the beta form) in the pregnant cow. Meyer (1992) reported the pre...
Application of high-performance liquid chromatography–inductively coupled plasma mass spectrometry to the investigation of cadmium speciation in pig kidney following cooking and in vitro gastro-intestinal digestion. The speciation of cadmium in retail pig kidney has been examined by size-exclusion chromatography (SEC) coupled directly to inductively coupled plasma mass spectrometry (ICP-MS). Approximately 35% of the cadmium from uncooked kidney was soluble after aqueous extraction at pH 8 and SEC - ICP-MS revealed three discrete peaks whose retention times corresponded to estimated relative molecular masses of 1.2 x 10(6), 7.0 x 10(4) and 6 x 10(3)-9 x 10(3). In the cooked kidney, 35% of the Cd was soluble and was all associated with a peak of a relative molecular mass (Mr) of 6 x 10(3)-9 x 10(3). After s...
