RESUMEN
A 32-year-old male went to the police to claim he just killed his girlfriend by inflicting several stabs with a kitchen knife. He was very nervous and particularly aggressive. About 90 min after the assault, a blood specimen was collected with natrium fluoride as preservative. The blood was free of alcohol, pharmaceuticals and drugs of abuse, but tested positive by LC-MS/MS for metandienone (32 ng/mL) and trenbolone (9 ng/mL). The perpetrator admitted regular consumption of anabolic steroids to enhance his muscular mass, as he was a professional security agent. To document long-term steroid abuse, a hair specimen was collected 3 weeks after the assault, which tested positive for both drugs. Segmental analyses revealed in the proximal 1.5 cm segment, corresponding to the period of the assault, the simultaneous presence of metandienone (11 pg/mg) and trenbolone (14 pg/mg), while only metandienone (3 pg/mg) was identified in the distal 1.5 cm segment. As aggressiveness and violence can be associated with abuse of anabolic steroids, the aetiology of this domestic crime was listed to be due impulsive behaviour in a context of antisocial lifestyle.
Asunto(s)
Anabolizantes/análisis , Metandrostenolona/análisis , Detección de Abuso de Sustancias , Congéneres de la Testosterona/análisis , Acetato de Trembolona/análisis , Adulto , Anabolizantes/efectos adversos , Análisis Químico de la Sangre , Análisis de Cabello , Homicidio/psicología , Humanos , Masculino , Metandrostenolona/efectos adversos , Trastornos Relacionados con Sustancias/psicología , Congéneres de la Testosterona/efectos adversos , Acetato de Trembolona/efectos adversos , Violencia/psicologíaRESUMEN
The current study represents a comprehensive investigation of the occurrence and fates of trenbolone acetate (TBA) and metabolites 17α-trenbolone (17α-TBOH), 17ß-TBOH, and trendione (TBO); melengesterol acetate (MGA); and the less commonly studied ß-andrenergic agonist ractopamine (RAC) in two 8 month cattle feeding trials and simulated rainfall runoff experiments. Cattle were administered TBA, MGA, or RAC, and their residues were measured in fresh feces, pen floor material, and simulated rainfall runoff from pen floor surfaces and manure-amended pasture. Concentrations of RAC ranged from 3600 ng g-1, dry weight (dw), in pen floor to 58â¯000 ng g-1 in fresh feces and were, on average, observed at 3-4 orders of magnitude greater than those of TBA and MGA. RAC persisted in pen floors (manure t1/2 = 18-49 days), and contamination of adjacent sites was observed, likely via transport of windblown particulates. Concentrations in runoff water from pen floors extrapolated to larger-scale commercial feedlots revealed that a single rainfall event could result in mobilization of gram quantities of RAC. This is the first report of RAC occurrence and fate in cattle feedlot environments, and will help understand the risks posed by this chemical and inform appropriate manure-management practices.
Asunto(s)
Contaminantes del Suelo , Animales , Bovinos , Estiércol , Fenetilaminas , Acetato de Trembolona/análisisRESUMEN
Photolysis of trenbolone acetate (TBA) metabolites in the presence of various nitrogen-, sulfur-, or oxygen-containing nucleophiles (e.g., azide, ammonia, or thiosulfate, respectively) results in rapid (half-lives â¼20-60 min), photochemically induced nucleophile incorporation across the parent steroid's trienone moiety. The formation of such nucleophile adducts limits formation of photohydrates, suggesting competition between the nucleophile and water for photochemical addition into the activated steroid structure. Analogous to previously reported photohydration outcomes, LC/MS analyses suggest that such photonucleophilic addition reactions are reversible, with more rapid elimination rates than thermal dehydration of photohydrates, and regenerate parent steroid structures. Beyond photonucleophilic addition pathways, we also found that hydroxylamine and presumed nucleophilic moieties in model dissolved organic matter (DOM; Fluka humic acid) can react via thermal substitution with TBA metabolite photohydrates, although this reaction with model DOM was only observed for photohydrates of trendione. Most nucleophile addition products [i.e., formed via (photo)reaction with thiosulfate, hydroxylamine, and ammonia] are notably more polar relative to the parent metabolite and photohydration products. Thus, if present, both nucleophilic adducts and bound residues in organic matter will facilitate transport and help mask detection of TBA metabolites in surface waters and treatment systems.
Asunto(s)
Acetato de Trembolona , Contaminantes Químicos del Agua , Cromatografía Liquida , Sustancias Húmicas , Espectrometría de Masas , Fotólisis , Acetato de Trembolona/análisisRESUMEN
A quick, easy, cheap, effective, rugged, and safe QuEChERS (method) was used for the simultaneous detection of four veterinary drug residues, namely naloxone, yohimbine, thiophanate, and altrenogest, in porcine muscle, using liquid chromatography with electrospray ionization triple quadrupole tandem mass spectrometry. Because of the unavailability of a suitable internal standard, matrix-matched calibrations were used for quantification, with determination coefficients ≥ 0.9542. The accuracy (expressed as recovery %) ranged from 60.53 to 83.25%, and the intra- and interday precisions (expressed as relative standard deviations) were <12%. The limits of quantification were 5, 0.5, 2, and 5 ng/g for naloxone, yohimbine, thiophanate, and altrenogest, respectively. Samples purchased from local markets in Seoul, Republic of Korea, revealed no traces of the target analytes. The developed method described herein is sensitive and reliable and can be applied to quantify the tested veterinary drugs in animal tissues.
Asunto(s)
Residuos de Medicamentos/aislamiento & purificación , Músculos/química , Naloxona/aislamiento & purificación , Extracción en Fase Sólida/métodos , Tiofanato/aislamiento & purificación , Acetato de Trembolona/análogos & derivados , Drogas Veterinarias/aislamiento & purificación , Yohimbina/aislamiento & purificación , Animales , Cromatografía Líquida de Alta Presión , Residuos de Medicamentos/análisis , Contaminación de Alimentos/análisis , Límite de Detección , Carne/análisis , Naloxona/análisis , Porcinos , Espectrometría de Masas en Tándem , Tiofanato/análisis , Acetato de Trembolona/análisis , Acetato de Trembolona/aislamiento & purificación , Drogas Veterinarias/análisis , Yohimbina/análisisRESUMEN
Chemical pollution is a pervasive and insidious agent of environmental change. One class of chemical pollutant threatening ecosystems globally is the endocrine disrupting chemicals (EDCs). The capacity of EDCs to disrupt development and reproduction is well established, but their effects on behaviour have received far less attention. Here, we investigate the impact of a widespread androgenic EDC on reproductive behaviour in the guppy, Poecilia reticulata. We found that short-term exposure of male guppies to an environmentally relevant concentration of 17ß-trenbolone-a common environmental pollutant associated with livestock production-influenced the amount of male courtship and forced copulatory behaviour (sneaking) performed toward females, as well as the receptivity of females toward exposed males. Exposure to 17ß-trenbolone was also associated with greater male mass. However, no effect of female exposure to 17ß-trenbolone was detected on female reproductive behaviour, indicating sex-specific vulnerability at this dosage. Our study is the first to show altered male reproductive behaviour following exposure to an environmentally realistic concentration of 17ß-trenbolone, demonstrating the possibility of widespread disruption of mating systems of aquatic organisms by common agricultural contaminants.
Asunto(s)
Agricultura , Conducta Sexual Animal/efectos de los fármacos , Contaminantes Químicos del Agua/efectos adversos , Contaminación del Agua/efectos adversos , Andrógenos/análisis , Andrógenos/farmacología , Animales , Peso Corporal/efectos de los fármacos , Disruptores Endocrinos/efectos adversos , Femenino , Masculino , Pigmentación/efectos de los fármacos , Poecilia , Caracteres Sexuales , Acetato de Trembolona/análisis , Acetato de Trembolona/farmacologíaRESUMEN
A rapid liquid chromatography tandem mass spectrometry method has been developed and validated for the determination of α-trenbolone, ß-trenbolone, α-nortestosterone, ß-nortestosterone, zeranol, and taleranol in bovine liver. The impact of liquid-liquid extraction with methyl tert-butyl ether and optimized solid phase extraction on silica cartridges significantly reduced effort and time of sample preparation. Electrospray ionization gives a significant signal increase compared with atmospheric pressure chemical ionization and atmospheric pressure photoionization. The HPLC gradient was optimized to separate isobaric analytes and matrix constituents from the hormone molecules. The optimized time and temperature of enzymatic hydrolysis of conjugated trenbolone was 4 h at 52 °C. The method validated in the range of 0.5-30 µg kg(-1) for α-trenbolone, ß-trenbolone, zeranol, taleranol, and 2-30 µg kg(-1) for α-nortestosterone, ß-nortestosterone. Combined uncertainty of measurements was in the range of 4%-23%. The matrix effect was negligible (1%-5%) for all analytes except of α-nortestosterone (19%). The developed method with changes concerning sample size and hydrolysis was also applied for the analysis of meat, serum, and urine samples. Graphical Abstract Determination of trenbolone, nortestosterone and zeranol in bovine liver.
Asunto(s)
Anabolizantes/análisis , Estrógenos no Esteroides/análisis , Hígado/química , Nandrolona/análisis , Acetato de Trembolona/análisis , Zeranol/análisis , Animales , Bovinos , Cromatografía Líquida de Alta Presión/métodos , Límite de Detección , Extracción Líquido-Líquido/métodos , Éteres Metílicos , Espectrometría de Masas en Tándem/métodos , Zearalenona/análisisRESUMEN
To assess the relative ecological risks of trenbolone acetate (TBA) use in agro-ecosystems, we evaluated the spatiotemporal dynamics of TBA metabolite transport during irrigation and rainfall events. Within a pasture, TBA-implanted heifers (40 mg TBA, 8 mg estradiol) were briefly penned (24 h) at high stocking densities (500 animal units (AU)/ha), prior to irrigation. Irrigation runoff concentrations of 17α-trenbolone (17α-TBOH) 0.3 m downslope were 11 ng/L in the wetting front, but quickly decreased to â¼0.5 ng/L, suggesting mass transfer limitations to transport. At 3 and 30 m downslope, efficient attenuation of 17α-TBOH concentrations is best explained by infiltration and surface partitioning. At plot scales, transport through vegetated filter strips resulted in <0.5-7 ng/L 17α-TBOH concentrations in rainfall-induced runoff with partial subsequent attenuation. Thus, even under intense grazing scenarios, TBA-metabolite transport potential is expected to be low in rangelands, with ecological risks primarily arising from uncontrolled animal access to receiving waters. However, 17α-TBOH concentrations in initial runoff were predicted to exceed threshold levels (i.e., no observed adverse effect levels [NOAELs]) for manure concentrations exceeding 2.0 ng/g-dw, which occurs throughout most of the implant life. For comparison, estrone and 17ß-estradiol were modeled and are likely capable of exceeding NOAELs by a factor of â¼2-5 in irrigation runoff, suggesting that both endogenous and exogenous steroids contribute to endocrine disruption potential in agro-ecosystems.
Asunto(s)
Estradiol/análisis , Estrógenos/análisis , Estrona/análisis , Contaminantes del Suelo/análisis , Acetato de Trembolona/análogos & derivados , Acetato de Trembolona/análisis , Agricultura/métodos , Anabolizantes/análisis , Anabolizantes/farmacocinética , Animales , Bovinos , Estradiol/farmacocinética , Estrógenos/farmacocinética , Femenino , Estiércol/análisis , Modelos Teóricos , Lluvia , Acetato de Trembolona/farmacocinéticaRESUMEN
A 29-year-old man with no previous medical history was found dead at home. Anabolic products (tablets and oily solutions) and syringes were found at the scene. The man was known to train regularly at a fitness club and to use anabolic drugs. Following an unremarkable autopsy with normal histology, toxicological analyses were requested by the local prosecutor to provide further information. Blood, head hair (5 cm, black), body hair (axillary and leg) and toe and finger nail clippings were submitted to liquid and gas chromatography coupled to tandem mass spectrometry (LC and GC-MS-MS) methods to test for anabolic steroids. Blood tested positive for testosterone (4 ng/mL), boldenone (26 ng/mL), stanozolol (3 ng/mL) and trenbolone (<1 ng/mL). Segmental head hair tests (2 × 2.5 cm) revealed a repeated consumption of testosterone (65-72 pg/mg), testosterone propionate (930-691 pg/mg), testosterone isocaproate (79 pg/mg to <5 pg/mg), nandrolone decanoate (202-64 pg/mg), boldenone (16 pg/mg), stanozolol (575-670 pg/mg), trenbolone (4 pg/mg-not detected), drostanolone (112-30 pg/mg), drostanolone enanthate (26-5 pg/mg) and drostanolone propionate (15-4 pg/mg). In addition to the substances identified in head hair, testosterone decanoate, testosterone cypionate and nandrolone were identified in both body hair and nails. The experts concluded that the manner of death can be listed as toxic due to massive repetitive use of anabolic steroids during the previous months. For anabolic agents, blood does not seem to be the best matrix to document a fatal intoxication. Indeed, these products are toxics when abused long term and are known to cause cardiac, hepatic and renal diseases. When compared to blood, hair and nails have a much larger window of detection. Therefore, keratinous matrices seem to be the best approach to test for anabolic steroids when a sudden death is observed in the context of possible abuse of steroids.
Asunto(s)
Anabolizantes , Humanos , Adulto , Anabolizantes/análisis , Estanozolol/análisis , Queratinas/análisis , Acetato de Trembolona/análisis , Cromatografía de Gases y Espectrometría de Masas/métodos , Testosterona , Congéneres de la Testosterona/análisis , Cabello/químicaRESUMEN
Supplements and growth promotants containing steroid hormones are routinely administered to beef cattle to improve feeding efficiency, reduce behavioral problems, and enhance production. As a result, beef cattle manure will contain both synthetic steroids as well as a range of endogenous steroids including androgens, estrogens, and progestogens. A two-year controlled study was conducted in which beef cattle were administered steroid hormones via subcutaneous implants and feed additives and the occurrence of 16 endogenous and synthetic steroid hormones and metabolites was evaluated in runoff from beef cattle feedlots and in manure and soil collected from feedlot surfaces. Samples were extracted and analyzed using liquid chromatography tandem mass spectrometryfor metabolites of the synthetic androgen trenbolone acetate, 17α-trenbolone, 17ß-trenbolone, for the nonsteroidal semisynthetic estrogen agonist, α-zearalanol, and the synthetic progesterone melengesterol acetate, as well as a wide range of endogeneous estrogens, androgens, and fusarium metabolites. Synthetic steroids including trenbolone metabolites and melengestrol acetate were detected in fresh manure and in feedlot surface soils from cattle administered synthetic steroids at concentrations up to 55 ± 22 ng/g dry weight (dw) (17α-trenbolone) and 6.5 ± 0.4 ng/g dw (melengesterol acetate). Melengesterol acetate was detected in 6% of runoff samples from feedlots holding cattle administered synthetic steroids at concentrations ranging up to 115 ng/L. The presence of melengesterol acetate in runoff from beef cattle feeding operations has not been previously reported. Synthetic steroids were not detected in manure or runoff from control cattle. A wide range of endogenous hormones were detected in runoff and feedlot surface soils and manure from cattle given synthetic steroids and from control cattle, with no statistically significant differences in concentration. These results indicate that runoff from confined animal production facilities is of environmental and public health concern regardless of the use of growth promotants.
Asunto(s)
Agricultura/métodos , Suplementos Dietéticos/análisis , Monitoreo del Ambiente/estadística & datos numéricos , Hormonas Esteroides Gonadales/análisis , Estiércol/análisis , Contaminantes del Suelo/análisis , Contaminantes Químicos del Agua/análisis , Animales , Bovinos , Cromatografía Liquida , Monitoreo del Ambiente/métodos , Hormonas Esteroides Gonadales/agonistas , Sustancias de Crecimiento/análisis , Acetato de Melengestrol/análisis , Espectrometría de Masas en Tándem , Acetato de Trembolona/análisis , Zeranol/análisisRESUMEN
Manure is increasingly being viewed as a threat to aquatic ecosystems due to the introduction of natural and synthetic hormones from land application to agricultural fields. In the Midwestern United States, where most agricultural fields are tile-drained, there is little known about hormone release from fields receiving animal wastes. To this end, seven sampling stations (four in subsurface tile drains and three in the receiving ditch network) were installed at a Midwest farm where various types of animal wastes (beef, dairy, and poultry lagoon effluent, dairy solids, and subsurface injection of swine manure) are applied to agricultural fields. Water flow was continuously monitored and samples were collected for hormone analysis during storm events and baseline flow for a 15 month study period. The compounds analyzed included the natural hormones 17α- and 17ß-estradiol, estrone, estriol, testosterone, and androstenedione and the synthetic androgens 17α- and 17ß-trenbolone and trendione. Hormones were detected in at least 64% of the samples collected at each station, with estrone being detected the most frequently and estriol the least. Testosterone and androstendione were detected more frequently than synthetic androgens, which were detected in fewer than 15% of samples. Hormone concentrations in subsurface tile drains increased during effluent irrigation and storm events. Hormones also appeared to persist over the winter, with increased concentrations coinciding with early thaws and snowmelt from fields amended with manure solids. The highest concentration of synthetic androgens (168 ng/L) observed coincided with a snowmelt. The highest concentrations of hormones in the ditch waters (87 ng/L for total estrogens and 52 ng/L for natural androgens) were observed in June, which coincides with the early life stage development period of many aquatic species in the Midwest.
Asunto(s)
Hormonas/análisis , Eliminación de Residuos Líquidos , Contaminantes Químicos del Agua/análisis , Androstenodiona/análisis , Animales , Monitoreo del Ambiente , Estradiol/análisis , Estrenos/análisis , Estriol/análisis , Estrógenos/análisis , Estrona/análisis , Agua Subterránea , Estiércol , Testosterona/análisis , Acetato de Trembolona/análisisRESUMEN
An inexpensive, harmless, and quick technique of sample preparation followed by a reversed-phase high-performance liquid chromatography (HPLC) for the simultaneous quantification of trenbolone acetate and 17beta-trenbolone in cattle muscle is presented. Analysis by HPLC with photo-diode array detector was performed using a short C1 column with an isocratic mobile phase. The method was validated by the analyses of spiked samples, resulting recoveries (> or = 87.9%; relative standard deviations < or = 3.4%), analytical total time (< 20 min/sample, where, a batch of 12 samples in 2 h), and quantitation limits (< or = 1.8 ng/g). No harmful organic solvents and reagents were used at all.
Asunto(s)
Anabolizantes/análisis , Cromatografía Líquida de Alta Presión/métodos , Carne/análisis , Acetato de Trembolona/análogos & derivados , Animales , Bovinos , Contaminación de Alimentos/análisis , Músculo Esquelético/química , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Acetato de Trembolona/análisisRESUMEN
A sensitive method was developed and validated for the quantitation of trenbolone residues in bovine liver. Target analytes were extracted from liver homogenate using solid phase cartridges, separated on a Phenyl column and detected using an electrospray ionization mass spectrometer operating in positive ion mode. The mean recovery of the analytes was between 62% and 69%. The method provided detection capabilities of 1 microg/kg for trenbolone. The method is suitable for application in veterinary drug residue in surveillance programme.
Asunto(s)
Anabolizantes/análisis , Contaminación de Alimentos/análisis , Hígado/química , Espectrometría de Masa por Ionización de Electrospray/métodos , Detección de Abuso de Sustancias/métodos , Acetato de Trembolona/análisis , Animales , Bovinos , Cromatografía Líquida de Alta Presión , Drogas Veterinarias/análisisRESUMEN
Here, we developed a novel and sensitive method for the detection and quantification of metastable trenbolone and altrenogest photoproducts in agricultural receiving waters based on solid phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Primary method analytes were seven cycloaddition or photohydration transformation products of 17α-trenbolone (17α-TBOH), 17ß-trenbolone (17ß-TBOH), trendione (TBO), and altrenogest (ALT), which are key contributors to the fate and environmental risks of these steroidal pharmaceuticals. Because commercial analytical standards are not available, reference standards for photoproducts were generated from trenbolone or ALT with a solar simulator (Ë6â¯h, >10 half-lives). Efficient detection of metastable photoproducts required cold and pH neutral conditions, rapid sample processing, minimal sample storage, and consideration of cationic artifacts. Method detection limits (MDLs) were 0.034-0.40â¯ngâ¯L-1 for parent compounds and 0.16-2.1â¯ngâ¯L-1 for photoproducts, sufficient for their detection in agroecosystems. Matrix suppression was observed and corrected by internal standards, and relative recovery rates were near 100% for all analytes except for 12-OH-17α-TBOH (Ë75% recovery). Intra-day variation was <20% and inter-day variation <25% for all the analytes. The developed method is capable of the analysis of trenbolone, altrenogest, and their key bioactive photoproducts in agricultural receiving waters.
Asunto(s)
Cromatografía Liquida/métodos , Espectrometría de Masas en Tándem/métodos , Acetato de Trembolona/análogos & derivados , Acetato de Trembolona/análisis , Cationes , Luz , Límite de Detección , Reproducibilidad de los ResultadosRESUMEN
This study evaluated the sorption and transport potential of seven phototransformation products of 17α-trenbolone, 17ß-trenbolone, trendione, and altrenogest, along with the parent trienone steroids in batch and column soil-water systems. In batch systems, the target solutes exhibited linear isotherms, with values for sorption coefficients (log Koc) of parent steroids (2.46-2.76) higher than those for photoproducts (1.92-2.57). In column systems, the estimated retardation factors (Rsol) for parents (2.7-5.1) were â¼2-5 times higher than those for photoproducts (0.84-1.7). The log Koc (R2 = 0.75) and Rsol (R2 = 0.89-0.98) were well correlated with measured log Kow values, indicating that hydrophobic partitioning governed the soil-solute interaction of these biologically potent compounds in soil-water systems. These data indicated that photoproducts exhibited reduced sorption affinity and increased transport potential relative to more hydrophobic parent structures. In agroecosystems, traditional runoff management practices would be expected to exhibit reduced treatment effectiveness for photoproducts relative to the parent compounds of commonly used trienone steroids.
Asunto(s)
Contaminantes Ambientales/análisis , Estrenos/análisis , Acetato de Trembolona/análogos & derivados , Acetato de Trembolona/análisis , Adsorción , Agricultura , Contaminantes Ambientales/química , Estrenos/química , Modelos Químicos , Suelo/química , Acetato de Trembolona/química , Agua/químicaRESUMEN
The current study was undertaken to validate the performance for the determination of both TBA and beta-trenbolone (beta-TB) residues in porcine muscle at concentrations required to monitor compliance with the maximum residue limit (MRL). The method involves a one phase liquid-liquid extraction, cleanup with low-temperature fat precipitation, separation of the respective compounds by HPLC on a Capcell pak C(18) column, use of a methanol-water isocratic system as an eluent, and measurement by UV absorbance detection at 340 nm. Both compounds were confirmed using LC-MS/MS with electrospray interface (ESI) and a triple quadrupole (QqQ) analyzer. The method was found to be precise and accurate, with a linearity range of 1-10 microg/kg (r(2) >0.973). The intra- and interday precision showed good reproducibility with RSDs < or =13.25%. The LODs were 0.12 and 0.22 microg/kg, and the LOQs were 0.37 and 0.66 microg/kg, for TBA and beta-TB, respectively. The applicability of the method was demonstrated by analyzing real samples collected from major cities in the Republic of Korea. No residues of the selected compounds were detected in any of the samples. The advantages of our method are that it is: selective, sensitive, requires a short time for analysis (13 min), and performs simple sample extraction and clean-up procedure with low-temperature fat precipitation as compared to the previously published methods.
Asunto(s)
Anabolizantes/análisis , Cromatografía Líquida de Alta Presión/métodos , Residuos de Medicamentos/análisis , Músculo Esquelético/química , Espectrometría de Masa por Ionización de Electrospray/métodos , Espectrofotometría Ultravioleta/métodos , Espectrometría de Masas en Tándem/métodos , Acetato de Trembolona/análogos & derivados , Animales , Estándares de Referencia , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Porcinos , Acetato de Trembolona/análisisRESUMEN
Twenty heifers which were each administered 3 or 4 implants containing trenbolone acetate were slaughtered at 30 days post-implantation. Liquid chromatographic analyses were conducted on muscle collected from the rump, loin, shoulder, and neck, and on the liver of each animal. Residues present in liver were primarily 17alpha-trenbolone, and the residues found in the various muscle samples were primarily 17beta-trenbolone. The mean concentration of 17alpha-trenbolone in liver was 4.3 +/- 2.3 ng/g; the mean concentration of 17beta-trenbolone in muscle tissues was < 0.4 ng/g. There was a small but statistically significant effect of the number of implants used on the mean concentration of residues in loin muscles; animals with 3 trenbolone implants had higher mean residue concentrations than animals with 4 trenbolone implants. This suggests that, though the impact of implant numbers on the mean concentration of residues in muscle tissues is negligible relative to currently generally accepted maximum residue levels, mechanisms may exist for selective distribution and retention of residues within different muscle groups.
Asunto(s)
Anabolizantes/análisis , Anabolizantes/farmacocinética , Hígado/química , Músculo Esquelético/química , Acetato de Trembolona/análogos & derivados , Anabolizantes/administración & dosificación , Animales , Bovinos , Cromatografía Liquida/métodos , Implantes de Medicamentos , Femenino , Hígado/metabolismo , Músculo Esquelético/metabolismo , Extracción en Fase Sólida , Estereoisomerismo , Distribución Tisular , Acetato de Trembolona/administración & dosificación , Acetato de Trembolona/análisis , Acetato de Trembolona/farmacocinética , Drogas Veterinarias/administración & dosificación , Drogas Veterinarias/análisis , Drogas Veterinarias/farmacocinéticaRESUMEN
Tetrahydrogestrinone, gestrinone and trenbolone are synthetic 19-norsteroids with androgenic properties sharing a labile conjugated ketotrienyl motif. Their LC-MS analyses tend to overcome classical derivatization problems, a shortcoming to the use of GC-MS. Therefore, alternative derivatization procedures were evaluated. The procedure with methoxylamine: pyridine followed by TMSImid: MSTFA gave the best results. This is attributed to the stability of the MO-TMS derivatives hindering the formation of artifacts and tautomerism. A full method is presented including SPE, hydrolysis and liquid-liquid extraction. It was possible to confirm the analytes below 2 ng/mL in urine, being the method robust and cost effective also for screening proposes.
Asunto(s)
Cromatografía de Gases y Espectrometría de Masas/métodos , Gestrinona/análogos & derivados , Gestrinona/orina , Acetato de Trembolona/orina , Adulto , Femenino , Gestrinona/análisis , Gestrinona/química , Humanos , Estructura Molecular , Reproducibilidad de los Resultados , Acetato de Trembolona/análisis , Acetato de Trembolona/químicaRESUMEN
A specific and sensitive method based on liquid chromatography-tandem mass spectrometry using atmospheric pressure chemical ionization (LC-APCI-MS/MS) has been developed for the determination of four anabolic steroids [trenbolone, methylboldenone, methyltestosterone, and norethandrolone] in bovine muscle. Methyltestosterone- d 3 was used as internal standard. The procedure involved enzymatic hydrolysis, extraction with tert-butyl methyl ether, defattening, and final cleanup with solid-phase extraction with Oasis HLB cartridges. The analytes were analyzed by reversed-phase LC-MS/MS, acquiring two diagnostic product ions from the chosen precursor [M + H] (+) for the unambiguous confirmation of hormones. The method was validated according to the European Commission Decision 2002/657/EC for the detection and confirmation of residues in products of animal origin. The limits of detection (LOD) and limits of quantitation (LOQ) were found to be 0.3 ng/g and 1.0 ng/g, respectively. The accuracy and precision have been determined, with recoveries ranging from 83% to 104% and the CV factor not exceeding the value of 7%. The decision limits CCalpha were calculated and ranged from 0.05 to 0.15 ng/g while the detection capabilities CCbeta ranged from 0.09 to 0.25 ng/g. The method proved to be sensitive and reliable and thus renders an appropriate means for residue analysis studies.
Asunto(s)
Anabolizantes/análisis , Cromatografía Líquida de Alta Presión , Espectrometría de Masas , Músculos/química , Animales , Bovinos , Femenino , Masculino , Metiltestosterona/análisis , Noretandrolona/análisis , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Testosterona/análogos & derivados , Testosterona/análisis , Acetato de Trembolona/análisisRESUMEN
One of the principal metabolites in cattle excreta following the administration of Synovex® ONE, which contains estradiol benzoate and trenbolone acetate, is 17α-estradiol. As part of the environmental assessment of the use of Synovex ONE, data were generated to characterize the fate of 17α-estradiol in the environment. Studies were conducted to determine the degradation and transformation of 17α-[14 C]-estradiol in 2 representative water-sediment systems each under aerobic and anaerobic conditions. The same transformation products-estriol, 17ß-estradiol, and estrone-were formed, principally in the sediment phase, under both conditions in both systems. From the production of these transformation products, the 50% disappearance time (DT50) values of estrone and 17ß-estradiol were determined, along with the DT50 values of 17α-estradiol and the total drug (17α-estradiol + 17ß-estradiol + estrone). The results indicate that 17 α-[14 C]-estradiol was more persistent under anaerobic conditions than under aerobic conditions and that 17 α-[14 C]-estradiol was less persistent than its transformation products. The DT50 values for the total system (aqueous and sediment phases) and for the total residues (17α-estradiol, 17ß-estradiol, and estrone) were selected for use in modeling the environmental fate of estradiol benzoate. For aerobic degradation in the water-sediment system, the DT50 was 31.1 d, and it was 107.8 d for the anaerobic system. Environ Toxicol Chem 2017;36:621-629. © 2016 SETAC.
Asunto(s)
Monitoreo del Ambiente/métodos , Estradiol/análisis , Sedimentos Geológicos/química , Ríos/química , Contaminantes Químicos del Agua/análisis , Aerobiosis , Anaerobiosis , Animales , Biodegradación Ambiental , Bovinos , Estradiol/análogos & derivados , Estradiol/metabolismo , Estrona/análisis , Etinilestradiol/análisis , Etinilestradiol/metabolismo , Heces/química , Acetato de Trembolona/análisis , Acetato de Trembolona/metabolismo , Estados UnidosRESUMEN
Synovex® ONE is an extended-release implant containing the active ingredients estradiol benzoate and trenbolone acetate for use in beef steers and heifers. Trenbolone acetate is rapidly hydrolyzed in cattle to form 17ß-trenbolone and its isomer, 17α-trenbolone, which are further transformed to a secondary metabolite, trendione. As part of the environmental assessment for the use of Synovex ONE, data were generated to characterize the fate of 17α-trenbolone, which is the principal metabolite found in cattle excreta, in the environment. A study was conducted to determine the degradation and transformation of [14 C]-17α-trenbolone in 2 representative water-sediment systems under aerobic conditions. The same transformation products, 17ß-trenbolone and trendione, were formed, principally in the sediment phase, in both systems. From the production of these transformation products, the 50% disappearance time (DT50) values of 17ß-trenbolone and trendione were determined, along with the DT50 values of the parent compound and the total drug (17α-trenbolone + 17ß-trenbolone + trendione). The DT50 values for the total system (aqueous and sediment phase) and for the total residues (17α-trenbolone + 17ß-trenbolone + trendione) in the 2 systems were 34.7 d and 53.3 d, respectively. Environ Toxicol Chem 2017;36:630-635. © 2016 SETAC.