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1.
Food Chem Toxicol ; 144: 111603, 2020 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-32738380

RESUMO

Exposure to endocrine-disrupting compounds (EDCs) during pregnancy and early development can lead to adverse developmental outcomes in offspring. One of the endpoints of concern is feminization. The present study aimed to investigate for any possible correlations with endocrine sensitive parameters in the testes of male rat offspring following dam exposure to three EDCs by assessing the expression of endocrine-related genes. Dienestrol (DIES) [0.37-6.25 µg/kg bw/day], linuron (LIN) [1.5-50 mg/kg bw/day], flutamide (FLU) [3.5-50 mg/kg bw/day] as well as their binary mixtures were administered to sexually mature female rats from gestation day (GD) 6 until postnatal day (PND) 21. Gene expression analysis of Star, Cyp11a1, Cyp17a1, Hsd3b2, Pgr and Insl3 was performed by RT-qPCR. Administration of the anti-androgen FLU alone significantly upregulated Cyp11a1 and Cyp17a1 gene expression while administration of LIN and DIES alone did not alter significantly gene expression. The effects of the binary mixtures on gene expression were not as marked as those seen after single compound administrations. Deregulation of Cyp17a1 in rat pup testis, following administration of FLU alone or in mixtures to dams, was significantly correlated with the observed feminization endpoints in male pups.


Assuntos
Dienestrol/toxicidade , Flutamida/toxicidade , Regulação da Expressão Gênica/efeitos dos fármacos , Linurona/toxicidade , Exposição Materna , Testículo/efeitos dos fármacos , Animais , Sistema Enzimático do Citocromo P-450/genética , Feminino , Insulina/genética , Masculino , Gravidez , Efeitos Tardios da Exposição Pré-Natal , Proteínas/genética , Ratos , Testículo/metabolismo
2.
Food Chem Toxicol ; 139: 111256, 2020 May.
Artigo em Inglês | MEDLINE | ID: mdl-32171874

RESUMO

Exposure to endocrine-disrupting compounds (EDCs) during pregnancy can result in negative health effects in later generations, including sex changes and feminization. The present study assessed the feminization effects on male offspring rats of three EDCs: Dienestrol (DIES), Linuron (LIN), and Flutamide (FLU). Sexually mature female rats were exposed from gestation day (GD) 6 until postnatal day (PND) 21 to: 0.37, 0.75, 1.5, 3.12 or 6.25 µg/kg/day of DIES, 1.5, 3, 6, 12.5, 25 or 50 mg/kg/day of LIN, 3.5, 6.7, 12.5, 25 or 50 mg/kg/day of FLU, and the following mixtures: FLU + DIES (mg/kg/day+µg/kg/day), 3.5 + 0.37, or 3.5 + 3, 25 + 0.37, or 25 + 3; FLU + LIN (mg/kg/day + mg/kg/day), 3.5 + 12.5, or 25 + 12.5; and DIES + LIN (µg/kg/day + mg/kg/day), 0.37 + 12.5, or 3 + 12.5. Anogenital distance (AGD), nipple retention (NR) and cryptorchidism were evaluated. FLU produced a decrease of AGD, an increase of NR, and an increase of cryptorchidism at the highest dose. None of these three endpoints were significantly affected by LIN or DIES treatments alone. Combinations of FLU + LIN and FLU + DIES increased NR, and decreased AGD, while DIES + LIN did not produce any effects in male pups. Results show that FLU is able to induce feminization in male pups, while binary combinations of LIN and DIES did not modify the effects produced by FLU.


Assuntos
Dienestrol/toxicidade , Flutamida/toxicidade , Linurona/toxicidade , Exposição Materna/efeitos adversos , Animais , Animais Recém-Nascidos , Criptorquidismo/induzido quimicamente , Criptorquidismo/fisiopatologia , Relação Dose-Resposta a Droga , Determinação de Ponto Final , Feminino , Feminização/induzido quimicamente , Feminização/fisiopatologia , Masculino , Mamilos/anormalidades , Mamilos/efeitos dos fármacos , Tamanho do Órgão/efeitos dos fármacos , Gravidez , Efeitos Tardios da Exposição Pré-Natal/induzido quimicamente , Efeitos Tardios da Exposição Pré-Natal/fisiopatologia , Ratos , Ratos Sprague-Dawley , Testículo/anormalidades , Testículo/efeitos dos fármacos
3.
Mikrochim Acta ; 186(8): 525, 2019 07 10.
Artigo em Inglês | MEDLINE | ID: mdl-31292777

RESUMO

An electroanalytical method for determining dienestrol (DNL) in bovine urine samples is described. A glassy carbon electrode (GCE) modified with silver nanoparticles and functionalized multi-walled carbon nanotubes was used as working sensor. The modified GCE displays substantial analytical improvements including an amplified signal, fast electron transfer kinetics, and resistance to fouling. The irreversible oxidation signal of DNL is pH-dependent. Best reactivity is found at pH 3.0, where a typical anodic peak is recorded at 0.8 V (vs. Ag/AgCl). Square-wave voltammetry revealed a 8.4 nM detection limit (1.9 µg L-1), good repeatability and reproducibility (RSDs <5.0%), and good accuracy (93.2-99.4% recovery from spiked samples). The modified electrode is highly stable even in the presence of ions (Na+ and K+), urea and uric acid. The electrochemical sensor fulfills all requisites to be used as forensic device in surveillance of illegal livestock practices. Graphical abstract Schematic presentation of the construction of a glassy carbon electrode modified with silver nanoparticles and functionalized multi-walled carbon nanotubes. This sensor exhibited a remarkable performance for voltammetric detection of the illicit growth promoter dienestrol in animal urine.


Assuntos
Dienestrol/urina , Drogas Ilícitas/urina , Nanopartículas Metálicas/química , Nanotubos de Carbono/química , Prata/química , Animais , Bovinos , Dienestrol/química , Técnicas Eletroquímicas , Eletrodos , Drogas Ilícitas/química
4.
Food Chem Toxicol ; 128: 193-201, 2019 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-30986439

RESUMO

This study was aimed at determining whether dienestrol (DIES) affects reproduction in male offspring of rats following oral maternal exposure during gestation and lactation. Pregnant rats were treated from GD 6 to PND 21. Animals received 0 (control-vehicle), 0.75, 1.5, 3.12, 6.25, 12.5, 50, 75 µg/kg bw/d of DIES. A control group -without vehicle-was also included. High DIES concentrations caused abortions at 75 and 50 µg/kg bw/d, while at 12.5 µg/kg bw/d had still miscarriages. Ten male rats per group were kept alive until PND 90 to ensure sexual maturity. Body and organ weights, anogenital distance (AGD) at PNDs 21 and 90, biochemical and sperm parameters like motility, viability, morphology, spermatozoa and resistant spermatid counts, and histopathology for sexual organs and liver were determined. An increase in organ weight (liver and sexual organs) and a decrease in AGD due to vehicle were found. A reduction of sperm motility and viability, and an increase of abnormal sperm morphology were caused by DIES, which provoked a dose-dependent prostatitis. Maternal exposure to DIES induced toxicity on the reproductive system of the male offspring, which could affect the capacity of fertilization.


Assuntos
Dienestrol/toxicidade , Estrogênios não Esteroides/toxicidade , Genitália Masculina/efeitos dos fármacos , Exposição Materna , Motilidade Espermática/efeitos dos fármacos , Espermatozoides/efeitos dos fármacos , Aborto Animal/induzido quimicamente , Administração Oral , Animais , Peso Corporal/efeitos dos fármacos , Dienestrol/administração & dosagem , Relação Dose-Resposta a Droga , Estrogênios não Esteroides/administração & dosagem , Feminino , Masculino , Tamanho do Órgão/efeitos dos fármacos , Gravidez , Prostatite/induzido quimicamente , Ratos , Contagem de Espermatozoides
5.
Se Pu ; 36(6): 573-577, 2018 Jun 08.
Artigo em Chinês | MEDLINE | ID: mdl-30136480

RESUMO

A capillary electrophoresis (CE) method was developed for the simultaneous separation and determination of four phenolic estrogens (PEs), in which pressure-assisted electrokinetic injection (PAEKI) was adopted as the on-line concentration method to enrich the PEs. Several parameters affecting PAEKI conditions such as injection voltage and injection time, were systematically investigated and compared with the usual parameters. Under the optimized PAEKI conditions (-9 kV, 0.3 psi (ca. 2.1 kPa), 0.4 min), the four PEs separated completely within 7 min. Good linearities were attained in the range of 0.05-5 mg/L for hexestrol and dienestrol, and 0.1-10 mg/L for bisphenol A and diethylstilbestrol, with correlation coefficients (r) over 0.9936. The limits of detection (S/N=3) were 0.0071-0.017 mg/L, and enrichment factors ranged from 11 to 15 compared to normal hydrodynamic injection. The combined micellar electrokinetic chromatographic-PAEKI method developed was used to determine the PEs in tap water and lake water samples; limits of quantification (S/N=10) of 0.029-0.064 mg/L and 0.033-0.079 mg/L were attained, respectively, by the two sample types. Furthermore, recoveries ranged from 75.6% to 110.1% with relative standard deviations (n=5) within 4.6%-11.8%. To use this PAEKI method, researchers would only need to adjust the parameters of the CE apparatus to perform on-line enrichment of analytes, without using other reagents; this demonstrates the simplicity, rapidity, and highly automated nature of this method.


Assuntos
Compostos Benzidrílicos/análise , Água Potável/análise , Estrogênios/análise , Fenóis/análise , Cromatografia Capilar Eletrocinética Micelar , Dienestrol/análise , Dietilestilbestrol/análise , Eletroforese Capilar , Água Doce , Hexestrol/análise , Lagos
6.
J Chromatogr A ; 1469: 8-16, 2016 Oct 21.
Artigo em Inglês | MEDLINE | ID: mdl-27688174

RESUMO

Highly selective and efficient magnetic molecularly imprinted polymers (MMIPs) were prepared using Fe3O4@SiO2 as a magnetic supporter, 3-methacryloxypropyltrimethoxy-silane (MPS) as a silane coupling agent, DIS as a template, methacrylic acid (MAA) as a functional monomer and ethyleneglycol dimethacrylate (EGDMA) as a cross-linker for the extraction of trace residuals of the synthetic estrogen dienestrol (DIS) in seawater, which is a concern worldwide for its endocrine disruption and carcinogenic danger to human health. The obtained MMIPs were demonstrated to have spherical morphologies, core-shell structures, large binding capacities, high efficiency and selectivity. These were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and adsorption experiments. Owing to the specific binding sites, the MMIPs exhibited an almost three times higher adsorption capacity towards DIS (Qmax=4.68mgg-1) than magnetic molecularly non-imprinted polymers (MNIPs) (Qmax=1.72mgg-1). DIS in spiked seawater samples from the Weihai Bay of China was extracted and enriched by MMIPs, and satisfactory recoveries (87.3%-96.4%) with low relative standard deviation (RSD) values (2.03%-5.18%, n=5) were obtained. The limit of detection (LOD) of the method obtained was 0.16µgL-1, and the limit of quantitation was 0.52µgL-1 after MMIPs. No significant deterioration of the adsorption capacity of the MMIPs was observed after six rounds of regeneration. The results further demonstrated the applicability of the MMIPs method, a simple and straightforward method for the extraction and enrichment of DIS in seawater without any time-consuming procedures.


Assuntos
Dienestrol/isolamento & purificação , Congêneres do Estradiol/isolamento & purificação , Nanopartículas de Magnetita/química , Poluentes Químicos da Água/isolamento & purificação , Adsorção , China , Humanos , Limite de Detecção , Microscopia Eletrônica de Transmissão , Impressão Molecular , Água do Mar/química , Silanos/química , Dióxido de Silício/química , Microextração em Fase Sólida
7.
Anal Bioanal Chem ; 408(21): 5801-5809, 2016 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-27311954

RESUMO

The food safety supervision in aquatic products has raised public concern in recent years. In this study, a liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method for the simultaneous quantification and identification of four residues of the ever widely used analytes (including malachite green, leucomalachite green, diethylstilbestrol, and dienestrol) in aquaculture samples was developed. For sample preparation, a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was used, which was initially developed for pesticide residue analysis. For cleanup procedure, low-temperature cleanup method was combined with multiplug filtration cleanup (m-PFC) method based on multi-walled carbon nanotubes (MWCNTs). The volume of water, extraction solvent, cleanup sorbents, and m-PFC procedure were optimized for carp, striped bass, and giant salamander matrices. It was validated by analyzing four residues in each matrix spiked at three concentration levels of 0.5, 5, and 50 µg/kg (n = 5). The method was successfully validated according to the 2002/657/EC guidelines. After optimization, spike recoveries were within 73-106 % and <15 % relative standard deviations (RSDs) for all analytes in the tested matrices. Limits of quantification (LOQs) for the proposed method ranged from 0.10 to 0.50 µg/kg. Matrix-matched calibrations were performed with the coefficients of determination >0.998 between concentration levels of 0.5 and 200 µg/kg. The developed method was successfully applied to the determination of residues in market samples. Graphical abstract Flow chart of multi-plug filtration cleanup combined with low-temperature cleanup method.


Assuntos
Dietilestilbestrol/análise , Resíduos de Drogas/análise , Contaminação de Alimentos/análise , Nanotubos de Carbono/química , Corantes de Rosanilina/análise , Alimentos Marinhos/análise , Espectrometria de Massas em Tandem/métodos , Animais , Bass/metabolismo , Carpas/metabolismo , Cromatografia Líquida/métodos , Dienestrol/análise , Dienestrol/metabolismo , Dietilestilbestrol/metabolismo , Resíduos de Drogas/metabolismo , Limite de Detecção , Corantes de Rosanilina/metabolismo , Extração em Fase Sólida/métodos , Urodelos/metabolismo
8.
Artigo em Inglês | MEDLINE | ID: mdl-25188907

RESUMO

A novel analytical method employing solid-phase extraction (SPE) coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 30 hormones in anti-ageing functional foods (capsules, powders and tablets). The analytes were extracted with acetic acid-acetonitrile (1-99 v/v), methanol and acetone, respectively. The extract was purified using a combined column, followed by analyte detection with electrospray ionisation in positive- or negative-ion modes. The results indicated that the 30 compounds had good linear correlations in the range of 1-1000 µg kg⁻¹, and the correlation coefficients were above 0.99. The limits of detection (LOD) and limits of quantification (LOQ) were 0.03-2 and 0.1-5 µg kg⁻¹, respectively. The average recovery of 30 compounds at the three spiked levels varied from 74.7% to 124.1%, and the relative standard deviation (RSD) was 2.4-15.0%. This method was applied to the analysis of hormones in 14 real samples of which seven hormones (such as estrone, dienestrol) were detected in four samples, but the remainder of the hormones were not detected. The developed method is sensitive, efficient, reliable and applicable to real samples.


Assuntos
Antioxidantes/química , Suplementos Nutricionais/análise , Contaminação de Alimentos , Inspeção de Alimentos/métodos , Hormônios/análise , Senilidade Prematura/prevenção & controle , Métodos Analíticos de Preparação de Amostras , Antioxidantes/economia , Antioxidantes/normas , China , Cromatografia Líquida de Alta Pressão , Dienestrol/análise , Dienestrol/química , Suplementos Nutricionais/economia , Suplementos Nutricionais/normas , Estrogênios/análise , Estrogênios/química , Estrogênios não Esteroides/análise , Estrogênios não Esteroides/química , Estrona/análise , Estrona/química , Fidelidade a Diretrizes , Hormônios/química , Limite de Detecção , Estrutura Molecular , Reprodutibilidade dos Testes , Extração em Fase Sólida , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas em Tandem
9.
Se Pu ; 32(2): 194-7, 2014 Feb.
Artigo em Chinês | MEDLINE | ID: mdl-24822457

RESUMO

A method for the determination of diethylstilbestrol (DES), hexestrol (HEX) and dienestrol (DS) residues in drinking water was established by on-line solid phase extraction (SPE) coupled with high performance liquid chromatography (HPLC). The material synthesized on the base of sol-gel technology was employed as adsorbent. This material was prepared using 3-aminopropyltriethoxysilane (APTES) as the functional monomer, tetraethoxysilane (TEOS) as the crosslinking agent, and acetic acid as the initiator. The synthesized adsorbent showed outstanding property for the estrogen extraction. The estrogen can be caught effectively from water samples and the extraction can be achieved rapidly. Some important parameters, such as pH of sample solution, eluent solvents, loading flow rate, which might influence extraction efficiency, were optimized. The results indicated that the limit of detection (S/N = 3) of the developed method could reach 0.07-0.13 microg/L under the conditions of pH 7.0 of sample solution, methanol and 1% (v/v) acetic acid aqueous solution as the eluent solvent and the loading flow rate of 2 mL/min. The recoveries of the three estrogens from the water samples at three spiked levels ranged from 82.31% to 99.43% with RSD of 1.61%-7.15%. The method was simple, rapid, and suitable to detect the trace residues of estrogens in drinking water.


Assuntos
Água Potável/análise , Estrogênios/análise , Poluentes Químicos da Água/análise , Cromatografia Líquida de Alta Pressão , Dienestrol , Dietilestilbestrol , Hexestrol , Polimetil Metacrilato , Propilaminas , Silanos , Extração em Fase Sólida
10.
Artigo em Inglês | MEDLINE | ID: mdl-24636894

RESUMO

A sensitive analytical method based on packed-fiber solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry (PF SPE-HPLC-MS/MS) has been developed for determination of three synthetic stilbenes in milk. The stilbenes are extracted with acetonitrile, using sodium chloride, and purified with PF SPE using a cartridge containing electrospun polystyrene nanofibers. Parameters affecting the efficiency of PF SPE, such as pH and amount of salt, were optimized. Under optimal conditions, the limits of detection and quantification were 5-13pg/g and 15-37pg/g, respectively. Absolute recoveries varied between 60% and 85% at three different levels. The method was successfully applied for the determination of estrogenic stilbenes in a total of 69 milk samples. The method is sensitive and cost-effective in stilbene detection, and has potential in quality control of dairy products.


Assuntos
Dienestrol/análise , Dietilestilbestrol/análise , Hexestrol/análise , Leite/química , Extração em Fase Sólida/métodos , Animais , Cromatografia Líquida de Alta Pressão/métodos , Dienestrol/química , Dienestrol/isolamento & purificação , Dietilestilbestrol/química , Dietilestilbestrol/isolamento & purificação , Hexestrol/química , Hexestrol/isolamento & purificação , Limite de Detecção , Modelos Lineares , Reprodutibilidade dos Testes , Espectrometria de Massas em Tandem/métodos
11.
Se Pu ; 30(7): 665-71, 2012 Jul.
Artigo em Chinês | MEDLINE | ID: mdl-23189660

RESUMO

A rapid, sensitive and accurate method for the simultaneous determination of six phenolic environmental estrogens, i. e., bisphenol A (BPA), diethylstilbestrol (DES), dienestrol( DE), hexestrol (HEX), 4-( tert-octyl)-phenol (4-tOP) and 4-nonylphenol (4-NP) in bullfrog blood by dispersive solid-phase extraction-ultrafast liquid chromatography-tandem mass spectrometry (dSPE-UFLC-MS/MS) was established. After protein precipitation, bullfrog blood samples were cleaned-up by dSPE method with ethylenediamine-functionalized Fe3O4, magnetic polymers (EDA-MPs) as adsorbent. The effects of precipitation solvents, adsorption time and the amount of EDA-MPs used on the recoveries of six phenolic environmental estrogens were investigated in detail. Chromatographic separation was performed on a Shim-pack XR-ODS II analytical column (100 mm x 2.0 mm, 2.2 microm). The mass spectrometer was operated by using electrospray ion (ESI) source in the multiple reaction monitoring (MRM) mode. The results showed that the linearities were in the range of 0.5-100.0 microg/L with correlation coefficients (r2) not less than 0.999 6 for all the six phenolic environmental estrogens. The lim- its of quantification (LOQs) (S/N > 10) in bullfrog blood samples were between 0. 075 microg/L and 0.40 microg/L. The recoveries were between 95.0% and 110.0% at three spiked levels. The precision values expressed as relative standard deviations (RSDs) were in the range of 0.6%-6.3%. The developed method can be applied to the routine analysis of the six phenolic environmental estrogens in bullfrog blood samples.


Assuntos
Cromatografia Líquida/métodos , Poluentes Ambientais/sangue , Estrogênios não Esteroides/sangue , Fenóis/sangue , Espectrometria de Massas em Tandem/métodos , Animais , Compostos Benzidrílicos/sangue , Dienestrol/sangue , Dietilestilbestrol/sangue , Rana catesbeiana/sangue , Extração em Fase Sólida/métodos
12.
Se Pu ; 30(11): 1133-42, 2012 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-23451515

RESUMO

A new stir bar sorptive extraction (SBSE) coating based on molecularly imprinted polymer (MIP) with diethylstilbestrol as replaced template molecule was prepared. The influences of the contents of template molecule and monomer in the polymerization mixture on the extraction performance of MIP-SBSE were investigated thoroughly. The MIP was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to evaluate the usability of the new coating, the MIP-SBSE was combined with high performance liquid chromatography (HPLC) and diode array detector (DAD) with dienestrol (DS) and hexestrol (HS) as detected solutes. To achieve optimally selective extraction performance for DS and HS, several parameters, including extraction and desorption times, desorption solvent, ionic strength and pH value in sample matrix were investigated. The results showed that under the optimized experimental conditions, the present method has high selectivity and sensitivity. When drying-redissolving procedure was taken during sample preparation, the limits of detection for DS and HS were as low as 0.04 microg/L and 0.14 micorg/L, respectively. Good linearities were obtained for analytes with the correlation coefficients (R2) above 0.99. Finally, the proposed method was successfully applied to the determination of DS and HS in wastewater, honey and cow urine samples. The recoveries of spiked target compounds in real samples ranged from 61.3% to 120%. The developed method is simple, selective, sensitive and applicable for the analysis of trace DS and HS in complicated samples.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Dienestrol/análise , Hexestrol/análise , Impressão Molecular , Extração em Fase Sólida/métodos , Adsorção , Fracionamento Químico/métodos , Dienestrol/isolamento & purificação , Hexestrol/isolamento & purificação , Polímeros/química
13.
Wei Sheng Yan Jiu ; 41(6): 956-62, 2012 Nov.
Artigo em Chinês | MEDLINE | ID: mdl-23424876

RESUMO

OBJECTIVE: Developing a rapid and sensitive analytical method based on ultrafast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) with solid-phase extraction (SPE) for the simultaneous determination of nine estrogens (dienestrol, diethylstilbestrol, estrone, hexestrol, 17-alpha-estradiol, 17-beta-estradiol, estriol, 17alpha-ethinylestradiol and estradiol valerate) in eel. METHODS: After the sample was extracted by acetonitrile and cleaned by Waters Oasis HLB solid-phase extraction cartridge, the UFLC separation was performed on a Shim-pack XR-ODS II column (100 mm x 2.0 mm, 2.2 microm) with a linear gradient elution program of methanol solution containing 0.04% ammonia (v/v) and 0.04% ammonia aqueous solution (v/v) as the mobile phase. Electrospray ionization was applied and operated in the negative multiple reaction monitoring (MRM) mode. The quantitation was used by isotope internal standard dilution technique. RESULTS: The results showed that the limits of quantitation (LOQs, S/N(10) were in the range of 0.07-0.4 microg/kg, the calibration curves were in good linearities for the nine analytes in the range of 0.5-50.0 microg/L with the correlative coefficients (r2) more than 0.998, the recoveries were between 81.0% and 110.0% with the relative standard deviations (RSDs) of 1.92%-8.24%. Additional, the mass spectra characterization of the nine estrogens was discussed and the fragmentation pathways were speculated. CONCLUSION: The developed method is rapid, sensitive, specific and reproducible, and adapts not only to the simultaneous determination of the nine trace estrogens including the epimer of 17-alpha-estradiol and 17-beta-estradiol but also to the identified detection in other fish tissues.


Assuntos
Cromatografia Líquida/métodos , Enguias , Estrogênios/análise , Produtos Pesqueiros/análise , Espectrometria de Massas em Tandem/métodos , Animais , Dienestrol/análise , Dietilestilbestrol/análise , Estrona/análise , Contaminação de Alimentos/análise , Técnica de Diluição de Radioisótopos , Extração em Fase Sólida/métodos
14.
Analyst ; 136(23): 5030-7, 2011 Dec 07.
Artigo em Inglês | MEDLINE | ID: mdl-21994916

RESUMO

A simple, rapid and sensitive method for the determination of diethylstilbestrol (DES), dienestrol (DE) and hexestrol (HEX) was developed by using the Nylon 6 nanofibers mat-based solid-phase extraction (SPE) coupled with liquid chromatography-tandem mass spectrometry (LC-MS). These estrogens were separated within 8 min by LC using an ODS column and methanol/water (80/20, v/v) at a flow rate of 1.0 mL min(-1). Electrospray ionization conditions in the negative ion mode were optimized for MS detection of the estrogens. Under the optimum SPE conditions, all target analytes in 50 mL environmental water samples can be completely extracted by 1.5 mg Nylon 6 nanofibers mat at flow rate of 3.0 mL min(-1) and easily eluted by passage of 500 µL mobile phase. By using the novel SPE-LC/MS method, good linearity of the calibration curve (r(2) ≥ 0.9992) was obtained in the concentration range from 0.10 ng L(-1) to 1.0 mg L(-1) (except for DE which was 0.20 ng L(-1) to 1.0 mg L(-1)) for all analytes examined. The limits of detection (S/N = 3) of the three estrogens ranged from 0.05 ng L(-1) to 0.10 ng L(-1). This method was applied successfully to the analysis of environmental water samples without any other pretreatment and interference peaks. Several water samples were collected from Jinchuan River and Xuanwu Lake, and in Jinchuan River water DES was detected at 0.13 ng L(-1). The recoveries of estrogens spiked into tap water were above 98.2%, and the relative standard deviations were below 4.78%.


Assuntos
Dienestrol/análise , Dietilestilbestrol/análise , Hexestrol/análise , Lagos/análise , Nanofibras , Rios/química , Poluentes Químicos da Água/análise , Caprolactama/análogos & derivados , Cromatografia Líquida/métodos , Dienestrol/isolamento & purificação , Dietilestilbestrol/isolamento & purificação , Hexestrol/isolamento & purificação , Lagos/química , Espectrometria de Massas/métodos , Polímeros , Extração em Fase Sólida/métodos
15.
BMC Cancer ; 9: 358, 2009 Oct 07.
Artigo em Inglês | MEDLINE | ID: mdl-19811643

RESUMO

BACKGROUND: Monomeric Group IVB (Ti, Zr and Hf) metallocenes represent a new class of antitumor compounds. There is literature on the general biological activities of some organotin compounds. Unfortunately, there is little information with respect to the molecular level activity of these organotin compounds. We recently started focusing on the anti-cancer activity of organotin polymers that we had made for other purposes and as part of our platinum anti-cancer effort. METHODS: For this study, we synthesized a new series of metallocene-containing compounds coupling the metallocene unit with dienestrol, a synthetic, nonsteroidal estrogen. This is part of our effort to couple known moieties that offer antitumor activity with biologically active units hoping to increase the biological activity of the combination. The materials were confirmed to be polymeric using light scattering photometry and the structural repeat unit was verified employing matrix assisted laser desorption ionization mass spectrometry and infrared spectroscopy results. RESULTS: The polymers demonstrated the ability to suppress the growth of a series of tumor cell lines originating from breast, colon, prostrate, and lung cancers at concentrations generally lower than those required for inhibition of cell growth by the commonly used antitumor drug cisplatin. CONCLUSION: These drugs show great promise in vitro against a number of cancer cell lines and due to their polymeric nature will most likely be less toxic than currently used metal-containing drugs such as cisplatin. These drugs also offer several addition positive aspects. First, the reactants are commercially available so that additional synthetic steps are not needed. Second, synthesis of the polymer is rapid, occurring within about 15 seconds. Third, the interfacial synthetic system is already industrially employed in the synthesis of aromatic nylons and polycarbonates. Thus, the ability to synthesize large amounts of the drugs is straight forward.


Assuntos
Antineoplásicos/farmacologia , Proliferação de Células/efeitos dos fármacos , Dienestrol/farmacologia , Neoplasias/fisiopatologia , Compostos Organometálicos/farmacologia , Antineoplásicos/síntese química , Antineoplásicos/química , Linhagem Celular Tumoral , Dienestrol/química , Humanos , Neoplasias/tratamento farmacológico , Compostos Organometálicos/síntese química , Compostos Organometálicos/química
16.
Aviakosm Ekolog Med ; 41(6): 13-7, 2007.
Artigo em Russo | MEDLINE | ID: mdl-18350830

RESUMO

Experiments with rats deprived of support loading on hind limbs by tail-suspension showed that injection of hormones participating in bone metabolism impeded the development of tibial spongy osteopenia; also, normalization of longitudinal bone growth was observed in several cases. Investigations were aimed to evaluate the effectiveness of growth hormone, sex hormones, thyreoid hormones, calcitonin, CNS stimulating ephedrine and strychnine, and graded support loads. The best results were obtained after injection of calcitonin combined with sinestrol (synthetic analog of estradiol) and graded support loads which acted as initiators and amplifiers of hormonal effects. The combination of calcitonin, sinestrol and support loads prevented osteopenia and provided the normal bone growth in length during rat's suspension.


Assuntos
Conservadores da Densidade Óssea/uso terapêutico , Doenças Ósseas Metabólicas/tratamento farmacológico , Doenças Ósseas Metabólicas/etiologia , Calcitonina/uso terapêutico , Dienestrol/uso terapêutico , Estrogênios não Esteroides/uso terapêutico , Hormônio do Crescimento/deficiência , Hormônio do Crescimento/uso terapêutico , Atividade Motora , Anabolizantes/uso terapêutico , Animais , Doenças Ósseas Metabólicas/complicações , Hipocinesia/complicações , Nandrolona/análogos & derivados , Nandrolona/uso terapêutico , Decanoato de Nandrolona , Ratos
17.
Se Pu ; 24(5): 462-5, 2006 Sep.
Artigo em Chinês | MEDLINE | ID: mdl-17165538

RESUMO

A method has been developed to determine residual stilbenes such as diethylstilbestrol (DES), dienestrol (DIS) and hexestrol (HS) in animal tissues using solid phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS). The procedures for extraction, cleanup on an LC-Si solid phase extraction cartridge and derivatization of stilbenes were established and optimized. The analytes were detected by mass spectrometer with electron impact source in selected ion monitoring mode (EI/SIM), and quantified with an external standard calibration curve method. Linear calibration curves were obtained in the concentration ranges from 5 to 500 microg/L for HS and from 10 to 1000 microg/L for DES and DIS (the correlation coefficients were above 0.99). Recoveries of the stilbenes were 73.0%-86.5%, and the relative standard deviations were between 1.0% and 7.2%. The limits of detection were 0.30 microg/kg for cis-DES, 0.10 microg/kg for trans-DES and HS and 0.15 microg/kg for DIS in pork and swine liver.


Assuntos
Dienestrol/análise , Dietilestilbestrol/análise , Resíduos de Drogas/análise , Hexestrol/análise , Animais , Cromatografia Gasosa-Espectrometria de Massas , Extração em Fase Sólida
18.
Electrophoresis ; 26(12): 2342-50, 2005 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-15920782

RESUMO

An improved technique, pressurized capillary electrochromatography (pCEC) coupling with end-column amperometric detection (AD), was developed and used for the separation and determination of estrogens. The effects of pH value, composition of mobile phase, concentration of the surfactant sodium dodecyl sulfate (SDS) and applied voltage on separation were investigated. The electrochemical oxidation of diethylstilbestrol (DES), dienestrol (DE), and hexestrol (HEX) could be reliably monitored with a carbon electrode at 0.9 V (vs. Ag/AgCl). The pCEC analyses were performed on a capillary separation column packed with 3 microm C18 particles with an acetonitrile/water (31%: 69%) mobile phase containing Tris buffer (5 mmol/L, pH 4.5) and 4 mmol/L SDS. High voltage up to 12 kV reduced the retention time dramatically and still provided a baseline resolution. In addition, supplementary pressure prevented bubble formation and provided reliability and reproducibility of the pCEC performance. The detection limits for the three estrogens ranged from 1.2 to 2.2x10(-7) mol/L, about 10 20-fold lower than those obtained with pCEC-UV detection. To evaluate the feasibility and reliability of this system, the proposed pCEC-AD method was further demonstrated with fish muscle samples spiked with estrogens.


Assuntos
Cromatografia Líquida/métodos , Eletroforese Capilar/métodos , Estrogênios/análise , Acetonitrilas , Animais , Tampões (Química) , Dienestrol/isolamento & purificação , Dietilestilbestrol/isolamento & purificação , Eletroquímica , Peixes , Hexestrol/isolamento & purificação , Concentração de Íons de Hidrogênio , Microeletrodos , Músculos/química , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Dodecilsulfato de Sódio
19.
Steroids ; 70(3): 173-8, 2005 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-15763595

RESUMO

A method for the synthesis of 2-hydroxyestrone/estradiol, 4-hydroxyestrone/estradiol, 3'-hydroxydiethylstilbestrol, 3'-hydroxyhexestrol, and 3'-hydroxydienestrol is reported, in which 2-iodoxybenzoic acid (IBX) and the corresponding phenolic estrogen are reacted. Treatment of the natural estrogens, estrone/estradiol, with stoichiometric amounts of IBX in dimethylformamide initially yielded a mixture of estrone/estradiol-2,3- and -3,4-quinones, which were reduced in situ to the corresponding catechols by treatment with a 1 M aqueous solution of ascorbic acid. Chromatographic separation of the reaction products afforded 2- and 4-hydroxyestrone/estradiol in good overall yields (79%). In the case of the synthetic estrogens containing two identical phenolic rings, protection of one ring is a prerequisite for the synthesis of the monocatechol. Thus, diethylstilbestrol and dienestrol were protected at one phenol ring as their methyl ethers. The resulting monophenols were treated with stoichiometric amounts of IBX for 1 h, followed by treatment with 1 M aqueous ascorbic acid to obtain the corresponding catechols in more than 70% yield. Furthermore, the catechol of diethylstilbestrol, protected at one ring, was reduced by catalytic hydrogenation at the C3-C4 double bond to obtain 3'-hydroxyhexestrol in 90% yield. Removal of the protected methoxy groups of the synthetic estrogen catechols was carried out by treatment with a 1 M solution of boron tribromide in dichloromethane. This method is highly efficient for the preparative scale synthesis of catechols of both natural and synthetic estrogens.


Assuntos
Catecóis/química , Catecóis/síntese química , Estrogênios/química , Iodobenzoatos/farmacologia , Oxigênio/metabolismo , Boro/química , Brometos/química , Dienestrol/química , Dimetilformamida/química , Iodobenzenos , Modelos Químicos , Fenol/química , Fenóis/química , Quinonas/química , Fatores de Tempo
20.
Aviakosm Ekolog Med ; 39(6): 33-7, 2005.
Artigo em Russo | MEDLINE | ID: mdl-16536031

RESUMO

Effects of graduated (2-hr.) support loading, synestrol and myocalcic on the thyroid C-cells was evaluated with the immunocytochemistry and cytomorphometry techniques. Graduated support loading was shown to partially recondition degraded functioning of C-cells. Synestrol injection suppressed the stimulating effect of support loading; myocalcic had a little effect on the C-cell activity. Simultaneous injection of two substances cancelled out the stimulating effect of support loading.


Assuntos
Conservadores da Densidade Óssea/uso terapêutico , Doenças Ósseas Metabólicas/terapia , Calcitonina/uso terapêutico , Dienestrol/uso terapêutico , Estrogênios não Esteroides/uso terapêutico , Glândula Tireoide/patologia , Suporte de Carga/fisiologia , Animais , Conservadores da Densidade Óssea/administração & dosagem , Doenças Ósseas Metabólicas/metabolismo , Doenças Ósseas Metabólicas/patologia , Calcitonina/administração & dosagem , Calcitonina/biossíntese , Dienestrol/administração & dosagem , Modelos Animais de Doenças , Estrogênios não Esteroides/administração & dosagem , Feminino , Seguimentos , Injeções Intramusculares , Ratos , Glândula Tireoide/metabolismo , Resultado do Tratamento
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