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1.
Bol. latinoam. Caribe plantas med. aromát ; 18(5): 518-526, sept. 2019. tab, ilus
Artigo em Inglês | LILACS | ID: biblio-1008290

RESUMO

Valeriana amurensis Smir. ex Kom. widely distributed in the northeast region of China and some region in Russia and Korea, and its underground parts (roots and rhizomes) being used to cure nervous system diseases such as insomnia. The active components including the essential oil and iridoids of underground parts were investigated in different harvest periods in order to evaluate the quality for the roots and rhizomes of V. amurensis. The content of the essential oil was obtained by hydrodistillation and bornyl acetate in the oil was quantitated by GC-EI. The iridoids, valepotriates were determined by potentiometric titration and the main component, valtrate was quantitated by HPLC-UV. The factors of biomass were considered in the determination of collection period. Statistical analysis of results showed that, the highest content of the essential oil per plant was 22.69 µl in withering period and then 21.58 µl in fruit ripening period, while the highest contents of bornyl acetate, valepotriates and valtrate per plant were 2.82 mg, 31.90 mg and 0.98 mg in fruit ripening period separately. Fruit ripening period was decided as the best harvest period for the content of active constituents and output of drug, and it would provide scientific basis for the artificial cultivation of V. amurensis.


Valeriana amurensis Smir. ex Kom. Se distribuye ampliamente en la región noreste de China y en algunas regiones de Rusia y Corea, y sus partes subterráneas (raíces y rizomas) se utilizan para curar enfermedades del sistema nervioso como el insomnio. Se investigaron los componentes activos, incluidos el aceite esencial y los iridoides de las partes subterráneas de V. amurensis en diferentes períodos de cosecha para evaluar la calidad de las raíces y rizomas. El contenido del aceite esencial se obtuvo mediante hidrodestilación y el acetato de bornilo en el aceite se cuantificó por GC-EI. Los iridoides, valepotriatos se determinaron mediante valoración potenciométrica y el componente principal, el valtrato se cuantificó por HPLC-UV. Los factores de biomasa fueron considerados en la determinación del período de recolección. El análisis estadístico de los resultados mostró que el mayor contenido de aceite esencial por planta fue de 22,69 µl en el período de marchitación y luego de 21,58 µl en el período de maduración de la fruta, mientras que el mayor contenido de acetato de bornilo, valepotriatos y valtrato por planta fue de 2.82 mg, 31.90 mg y 0,98 mg, respectivamente, en el período de maduración de la fruta por separado. Se definió el período de maduración de la fruta como el mejor período de cosecha para el contenido de constituyentes activos y la producción de droga, lo cual proporcionaría una base científica para el cultivo artificial de V. amurensis.


Assuntos
Valeriana/química , Óleos Voláteis/química , Raízes de Plantas/química , Estações do Ano , Bornanos/análise , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas por Ionização por Electrospray , Rizoma/química , Iridoides/análise
2.
Artigo em Chinês | MEDLINE | ID: mdl-31495125

RESUMO

Objective: To investigate the characteristics of occupational exposure to polycyclic aromatic hydrocarbons (PAHs) in the workplace and for various types of work in a carbon enterprise based on the measurement data of various components of PAHs in the air from the workplace of the carbon enterprise, and to provide a scientific basis for protection against PAHs in this enterprise. Methods: In July 2017, a carbon enterprise in Shandong Province and its on-duty workers were chosen as subjects. On-site occupational hygiene investigation and high-performance liquid chromatography were used to investigate and determine the presence and concentrations of PAHs in various workshops and various types of work in the enterprise, and toxic equivalent quantity (TEQ) was used to evaluate the carcinogenic level of PAHs. Results: The components of PAHs with relatively high content in the air of the workplace in the carbon enterprise were fluoranthene, pyrene, benzanthracene, X, and benzo[a]pyrene, with mean concentrations of 1 485.66, 864.66, 805.35, 500.08, and 120.88 ng/m(3), respectively. There were significant differences between the three workshops in the concentrations of PAHs components (benzo[a]pyrene, benzanthracene, benzo[b]fluoranthene, benzo[k]fluoranthene, X, fluoranthene, pyrene, fluorene, indenopyrene, and anthracene) and total TEQ (P<0.05) . The total TEQ of PAHs in the molding workshop was significantly higher than that in other workshops (P<0.05) . There were significant differences between different types of work in the exposure to pyrene and fluoranthene and TEQ (P<0.05) . Shaking-table operators, moving-sieve operators, batching operators, fabric workers, and hot-oil stove workers had higher exposure levels of PAHs. The exposure concentrations of benzo[a]pyrene and benzanthracene were highly correlated with total TEQ. Conclusion: The concentration of PAHs in the working environment of the carbon enterprise is generally higher; benzo[a]pyrene and fluoranthene are the PAHs components against which special protective measures need to be taken; molding workshops are the workshops that are most seriously endangered by PAHs; shaking-table operators are the type of workers needing special protection against PAHs. The occupational hazards of PAHs in the carbon industry cannot be ignored, against which corresponding protective measures should be formulated based on their exposure characteristics.


Assuntos
Carcinógenos/análise , Exposição Ocupacional/análise , Hidrocarbonetos Policíclicos Aromáticos/análise , Benzo(a)Antracenos/análise , Benzo(a)pireno/análise , Carbono , Cromatografia Líquida de Alta Pressão , Humanos , Saúde do Trabalhador
3.
Int J Pharm Compd ; 23(5): 434-437, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31513544

RESUMO

In order to avoid fluid overload, the use of more concentrated drug solutions in intensive care units and obstetrics is common. The objective of this study was to quantify the physicochemical stability of a concentrated solution of salbutamol (albuterol) in polypropylene syringes during 30 days of storage at 5°C ± 3°C with protection from light. Four 50-mL syringes containing 0.060mg/mL of salbutamol (albuterol) in 0.9% NaCl were prepared and stored at 5°C ± 3°C with protection from light during 30 days of storage. Immediately after preparation and periodically during the storage, salbutamol (albuterol) concentrations were measured by an ultra-performance liquid chromatography. Spectrophotometric absorbance at different wavelengths, pH measurement, and microscopic observations were also performed. All solutions were physicochemically stable during the entire period of storage at 5°C ± 3°C: no color change, turbidity, precipitation or opacity, significant pH variations, or optic densities were observed in the solutions. No crystals were seen by microscopic analysis. Concentrations of salbutamol remained stable during the storage period. Solutions of salbutamol (albuterol) 0.060 mg/mL in syringes of 0.9% NaCl are physically and chemically stable for at least 30 days when stored in syringes at 5°C ± 3°C with protection from light and may be prepared in advance by a centralized intravenous additive service.


Assuntos
Obstetrícia , Polipropilenos/química , Seringas , Albuterol , Cromatografia Líquida de Alta Pressão , Unidades de Terapia Intensiva
4.
Fa Yi Xue Za Zhi ; 35(4): 411-418, 2019 Aug.
Artigo em Inglês, Chinês | MEDLINE | ID: mdl-31532148

RESUMO

Abstract: Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) rapid determination method for simultaneous analysis of 20 fentanyl-related substances in blood. Methods With fentanyl-D5 as an internal standard, the blood was extracted by liquid-liquid extraction (LLE), then separated with an ACQUITY UPLC HSS T3 chromatographic column, and finally 20 fentanyl-related substances were simultaneously analyzed with multiple reaction monitoring (MRM) mode. Results The limits of detection (LOD) of all compounds were 0.02-0.03 ng/mL, and the limits of quantitation (LOQ) were 0.05-0.2 ng/mL. Within the mass concentration range of 0.05-40 ng/mL, 20 fentanyl-related substances had a good linear relationship, and correlation coefficients were larger than 0.99. The accuracy of the method was 87.69%-114.68% and the extraction recovery rate was 85.35%-101.80%, and no significant matrix effect was observed. The established method was successfully applied to the detection of sufentanil in rat blood after sufentanil was injected. Sufentanil could still be detected in blood of rats 10 h after sufentanil injection. Conclusion The established method has the advantages of simple pretreatment, high sensitivity and good selectivity, and can be used for the determination of fentanyl-related substances in forensic toxicology analysis.


Assuntos
Cromatografia Líquida de Alta Pressão , Fentanila/sangue , Espectrometria de Massas em Tandem , Animais , Toxicologia Forense , Ratos , Reprodutibilidade dos Testes , Sufentanil/sangue
5.
Fa Yi Xue Za Zhi ; 35(4): 419-422, 2019 Aug.
Artigo em Inglês, Chinês | MEDLINE | ID: mdl-31532149

RESUMO

Abstract: Objective To develop a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of the content of 4-fluoromethamphetamine (4-FMA) in rat plasma, and to provide a methodological basis for the study of the toxicokinetics of 4-FMA in rats. Methods Rat plasma samples were added into internal standard methamphetamine (MA). Its proteins were precipitated with methanol and then separated with Poroshell 120 EC-C18 chromatographic column. A 0.1% formic acid aqueous solution and a 0.1% formic acid acetonitrile solution were used as the mobile phase at the flow rate of 0.4 mL/min. Electrospray ionization source was used for detection in the multiple reaction monitoring (MRM) mode. Results The linear relationship was good when the mass concentration of 4-FMA in plasma samples was in the range of 5-1 000 ng/mL (r>0.999). The limit of detection (LOD) was 3 ng/mL and the limit of quantification (LOQ) was 5 ng/mL. The accuracy was expressed as relative error (RE), and in the range of ±5%, the intra-day precision and inter-day precision (relative standard deviation, RSD) less than 9%, and the extraction recovery rate was more than 90%. The analysis and detection of plasma samples were completed within 2.5 min. Conclusion This study developed a HPLC-MS/MS method for the determination of 4-FMA in rat plasma samples. This method is accurate, rapid, simple and sensitive and can be applied to the study of toxicokinetics of 4-FMA.


Assuntos
Cromatografia Líquida de Alta Pressão , Metanfetamina/sangue , Espectrometria de Massas em Tandem , Animais , Limite de Detecção , Metanfetamina/análogos & derivados , Ratos , Reprodutibilidade dos Testes , Toxicocinética
6.
Int J Pharm Compd ; 23(5): 414-417, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31513540

RESUMO

Furosemide parenteral solutions are routinely used in our hospital. However, the stability in transparent syringes is unknown. In this study, transparent polypropylene syringes were filled with 8 mL and 50 mL of furosemide 5-mg/mL solution. The furosemide was analyzed by high-performance liquid chromatography and assays were performed up to 35 days of storage of the syringes at 4°C protected from light, plus 24 hours at 20°C exposed to daylight. In addition, the appearance and pH of the solutions were determined. A microbiological assay using tryptic soy broth was also performed. Both types of syringes remained colorless, clear, and free from visible particles throughout the study period. The pH did not change, and concentrations remained between 95% and 105% of the stated concentration. None of the syringes filled with culture media exhibited bacterial or fungal growth. In conclusion, ready-to-administer furosemide 5-mg/mL, 8-mL, and 50-mL polypropylene syringes are stable for up to 35 days when stored in a refrigerator at 4°C protected from light, plus 24 hours at 20°C unprotected from light. These results allow maximum storage time in stock and the ability of 24-hour continuous infusion at ambient room temperature without protecting the syringe against light.


Assuntos
Furosemida/química , Polipropilenos , Seringas , Cromatografia Líquida de Alta Pressão , Estabilidade de Medicamentos , Armazenamento de Medicamentos , Polipropilenos/química
7.
J Agric Food Chem ; 67(38): 10800-10812, 2019 Sep 25.
Artigo em Inglês | MEDLINE | ID: mdl-31490681

RESUMO

In this work, a highly efficient pesticide residue screening and quantification method was established using ultrahigh-performance liquid chromatography-tandem quadrupole time-of-flight mass spectrometry based on in-source fragmentation. Over 400 pesticides were tested, among which 96 pesticides displayed in-source fragmentation. A novel concept of in-source fragment fraction was proposed to evaluate the extent of in-source fragmentation, which was found to be chemical structure- and source parameter-dependent. A high-resolution MS/MS library containing 403 pesticides and 126 fragments was created and was applied for library searching of pesticide residues in vegetables and fruits. The introduction of in-source fragments effectively circumvented misannotation and occurrence of false negatives. The quantification ability for the fragments was validated in terms of recovery, linearity, and limit of quantification and its superiority to the parent pesticides was established. Finally, the proposed method was applied for the analysis of real samples and proficiency test samples, and false negative results were successfully avoided in the analysis.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Frutas/química , Resíduos de Praguicidas/química , Espectrometria de Massas em Tandem/métodos , Verduras/química , Contaminação de Alimentos/análise , Limite de Detecção
8.
J Agric Food Chem ; 67(38): 10782-10790, 2019 Sep 25.
Artigo em Inglês | MEDLINE | ID: mdl-31490683

RESUMO

Systematic investigation of cyproconazole, including absolute stereochemistry, fungicidal activity, quantification in two matrixes, and stereoselective degradation in cucumber, are conducted in this study. By virtue of vibrational circular dichroism (VCD) spectroscopy, absolute configurations of four stereoisomers were identified to be (2R,3R)-(+)-, (2R,3S)-(+)-, (2S,3S)-(-)-, and (2S,3R)-(-)-cyproconazoles. Then four stereoisomers exhibited stereoselective fungicidal activities against Fusarium graminearum Schw and Magnaporthe oryzae, and the order of fungicidal activity was (2S,3S)-(-)-stereoisomer > the stereoisomer mixture > (2S,3R)-(-)-stereoisomer > (2R,3R)-(+)-stereoisomer > (2R,3S)-(+)-stereoisomer. Moreover, chiral liquid chromatography-tandem mass spectrometry was used to identify and quantify cyproconazole stereoisomers in soil and cucumber matrixes. Good linearity (R2 ≥ 0.99) and recoveries (86.79-92.47%, RSD ≤ 3.94%) for them were achieved, individually. Furthermore, stereoselective degradation of four cyproconazole stereoisomers was observed in cucumber and the order of degradation rate was (2R,3R)-(+)-cyproconazole > (2S,3S)-(-)-cyproconazole > (2R,3S)-(+)-cyproconazole > (2S,3R)-(-)-cyproconazole. We envision that such systematic assessments of chiral fungicides at an enantiomeric level would provide valuable information in future studies involving enantioselective physiological, metabolic, and toxicological activities.


Assuntos
Fungicidas Industriais/química , Triazóis/química , Alternaria/efeitos dos fármacos , Alternaria/crescimento & desenvolvimento , Cromatografia Líquida de Alta Pressão , Cucumis sativus/química , Contaminação de Alimentos/análise , Fungicidas Industriais/farmacologia , Fusarium/efeitos dos fármacos , Fusarium/crescimento & desenvolvimento , Rhizoctonia/efeitos dos fármacos , Rhizoctonia/crescimento & desenvolvimento , Poluentes do Solo/química , Poluentes do Solo/farmacologia , Estereoisomerismo , Espectrometria de Massas em Tandem , Triazóis/farmacologia
9.
J Agric Food Chem ; 67(38): 10791-10799, 2019 Sep 25.
Artigo em Inglês | MEDLINE | ID: mdl-31497956

RESUMO

Very weak signals of fragment ions of nosiheptide could be observed using liquid chromatography-tandem mass spectrometry. The preparation of 4-hydroxymethyl-3-methyl-1H-indole-2-carboxylic acid (HMIA), a specific fragment of nosiheptide, by alkaline hydrolysis is described. HMIA showed a good mass spectrometric signal in negative electrospray ionization mode. In the new method, the nosiheptide residue in muscle tissue was hydrolyzed with sodium hydroxide aqueous solution; this was followed by cleanup using mixed mode cartridges. Identification and quantification of nosiheptide were carried out by analyzing HMIA in hydrolysate of muscles. Nosiheptide showed a good linear relationship (r > 0.996) in the calibration range of 2-500 µg/kg, and a low limit of quantification of 2 µg/kg was obtained in swine, chicken, and fish muscles. Recoveries of nosiheptide from spiked muscle samples were 85-108% with relative standard deviations less than 10%. The proposed method was successfully applied for the detection of the nosiheptide residue in medicated animal tissues samples.


Assuntos
Antibacterianos/química , Cromatografia Líquida de Alta Pressão/métodos , Resíduos de Drogas/química , Contaminação de Alimentos/análise , Carne/análise , Espectrometria de Massas em Tandem/métodos , Álcalis/química , Animais , Galinhas , Peixes , Hidrólise , Limite de Detecção , Músculos/química , Suínos , Tiazóis/química
10.
Chem Biol Interact ; 311: 108796, 2019 Sep 25.
Artigo em Inglês | MEDLINE | ID: mdl-31421116

RESUMO

Lambda-cyhalothrin (LCT) is a broad-spectrum pesticide widely used in agriculture throughout the world. This pesticide is considered a potential contaminant of surface and underground water as well as food, posing a risk to ecosystems and humans. In this sense, we decided to evaluate the activity of enzymes belonging to the purinergic system, which is linked with regulation of extracellular nucleotides and nucleosides, such as adenosine triphosphate (ATP) and adenosine (Ado) molecules involved in the regulation of inflammatory response. However, there are no data concerning the effects of LCT exposure on the purinergic system, where extracellular nucleotides act as signaling molecules. The aim of this study was to evaluate nucleotide hydrolysis by E-NTPDase (ecto-nucleoside triphosphate diphosphohydrolase), Ecto-NPP (ecto-nucleotide pyrophosphatase/phosphodiesterase), ecto-5'-nucleotidase and ecto-adenosine deaminase (E-ADA) in platelets and liver of adult rats on days 7, 30, 45 and 60 after daily gavage with 6.2 and 31.1 mg/kg bw of LCT. Gene expression patterns of NTPDases1-3 and 5'-nucleotidase were also determined in those tissues. In parallel, lambda-cyhalothrin metabolites [3-(2-chloro-3,3,3- trifluoroprop-1-enyl)-2,2-dimethyl-cyclopropane carboxylic acid (CFMP), 4-hydroxyphenoxybenzoic acid (4-OH-3-PBA), and 3-phenoxybenzoic acid (3-PBA)] were measured in plasma. Results showed that exposure rats to LCT caused a significant increase in the assessed enzymes activities. Gene expression pattern of ectonucleotidases further revealed a significant increase in E-NTPDase1, E-NTPDase2, and E-NTPDase3 mRNA levels after LCT administration at all times. A dose-dependent increase in LCT metabolite levels was also observed but there no significant variations in levels from weeks to week, suggesting steady-steady equilibrium. Correlation analyses revealed that LCT metabolites in the liver and plasma were positively correlated with the adenine nucleotides hydrolyzing enzyme, E-ADA and E-NPP activities in platelets and liver of rats exposed to lambda-cyhalothin. Our results show that LCT and its metabolites may affect purinergic enzymatic cascade and cause alterations in energy metabolism.


Assuntos
Plaquetas/efeitos dos fármacos , Regulação da Expressão Gênica/efeitos dos fármacos , Fígado/efeitos dos fármacos , Nitrilos/farmacologia , Nucleotidases/genética , Nucleosídeos de Purina/metabolismo , Piretrinas/farmacologia , Adenosina Desaminase/genética , Adenosina Desaminase/metabolismo , Adenosina Trifosfatases/genética , Adenosina Trifosfatases/metabolismo , Animais , Plaquetas/enzimologia , Plaquetas/metabolismo , Cromatografia Líquida de Alta Pressão , Hidrólise , Fígado/enzimologia , Fígado/metabolismo , Masculino , Espectrometria de Massas , Nitrilos/sangue , Nitrilos/metabolismo , Nucleotidases/metabolismo , Piretrinas/sangue , Piretrinas/metabolismo , Pirofosfatases/genética , Pirofosfatases/metabolismo , Ratos , Ratos Wistar
12.
Sud Med Ekspert ; 62(4): 47-54, 2019.
Artigo em Russo | MEDLINE | ID: mdl-31407706

RESUMO

The purpose of the work is to determine the optimal conditions for isolating amlodipine, to purify it by the method of column chromatography and to develop a method for detecting it in biological material. TLC, GC-MS, low pressure column chromatography, and HPLC were used for analysis. We studied the comparative isolation of amlodipine from biological material using 13 isolating agents of organic nature, water, and aqueous solutions. The use of acetone as an insulating agent for the extraction of amlodipine from tissues of cadaver organs has been substantiated. The possibility of purification of the analyzed compound from the endogenous substances of the biomaterial is shown by the method of reversed phase chromatography in a column of the Silasorp S-18 sorbent of 30 µm. A technique has been developed for detecting amlodipine in the tissues of cadaveric organs (liver), which corresponds to the necessary parameters of linearity, selectivity, accuracy, precision and stability. The limits of detection and quantification of amlodipine by the proposed method are 0.25·10-6 and 4.0·10-6 g, respectively, in 1 g of the biomaterial.


Assuntos
Acetona , Anlodipino/isolamento & purificação , Cadáver , Cromatografia Líquida de Alta Pressão , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Reprodutibilidade dos Testes
13.
BMC Vet Res ; 15(1): 270, 2019 Aug 01.
Artigo em Inglês | MEDLINE | ID: mdl-31370899

RESUMO

BACKGROUND: Osteoarthritis is a common canine disease frequently treated with nutritional supplements that often lack independent verification of ingredients, active ingredient concentration, efficacy, or safety. Human supplements containing Boswellia serrata extracts (BSE) with high concentrations of active constituents 3-acetyl-11-keto-ß-boswellic acid (AKBA) and 11-keto-ß-boswellic acid (KBA) are bioavailable, safe, and efficacious in the alleviation of symptoms of naturally occurring osteoarthritis in people. Thus, oral AKBA and/or KBA supplementation could be a promising novel therapy for dogs with osteoarthritis. The primary objective of this study was to determine the concentrations of AKBA and KBA within six human and seven canine market formulations containing BSE administered to dogs, using a derivation of the previously validated high performance liquid chromatography (HPLC) method. The secondary objective was to compare measured concentrations to label claims. RESULTS: The mean concentrations of AKBA and KBA within the formulations tested were 42.3 mg/g AF (0.1-155.7 mg/g AF) and 5.2 mg/g AF (0-24.8 mg/g AF), respectively, with four of the formulations containing an undetectable amount of KBA. None of the market formulations had a label claim for KBA. For the five tested formulations with a label claim for AKBA, the mean percentage of detected AKBA was 173% of the concentration listed on the label (range: 114-224%). Formulations claiming to contain AKBA had a mean AKBA concentration of 98.2 mg/g AF, significantly higher than formulations claiming only to contain BSE (7.4 mg/g AF; p = 0.01). CONCLUSIONS: This study demonstrated a large variation of boswellic acid concentrations in market formulations claiming to contain BSE, with products claiming to contain AKBA containing higher concentrations of AKBA than other products. There was also a large variation in, and overall high, percent difference between label claims and measured concentrations of AKBA. All products met or exceeded label claims. However, differences between label amounts and detected concentrations confirm the need for independent laboratories to quantify concentrations of active ingredients in supplements containing BSE. This would be necessary prior to the use of these formulations in the research or clinical setting.


Assuntos
Boswellia/química , Suplementos Nutricionais/análise , Extratos Vegetais/química , Triterpenos/análise , Animais , Cromatografia Líquida de Alta Pressão , Cães
14.
Chem Pharm Bull (Tokyo) ; 67(8): 810-815, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31366830

RESUMO

Helicobacter pylori (H. pylori) infection is common and can result in gastric and duodenal ulcers, and in some cases, gastric lymphoma and cancer. Omeprazole (OMP)-in combination with clarithromycin (CLR), amoxicillin (AMX), tinidazole (TND), or metronidazole (MET)-is used in double or triple combination therapy for eradication of H. pylori. However, the roles of the drugs other than OMP are not clearly understood. Therefore, in the present study, we aimed to investigate any effects of these drugs on OMP metabolism by wild-type CYP2C19 using spectroscopy and enzyme kinetics. The dissociation constants (Kd) for CYP2C19 with OMP, CLR, AMX, TND, and MET were 8.6, 126, 156, 174, and 249 µM, respectively. The intrinsic clearance of OMP was determined to be 355 mL/min/µmol of CYP2C19. Metabolism of OMP was significantly inhibited by 69, 66, 28, and 40% in the presence of CLR, TND, AMX, and MET, respectively. Moreover, the combination of CLR and TND resulted in 76% inhibition of OMP metabolism, while the combination of AMX and MET resulted in 48% inhibition of OMP metabolism. Both combinations of drugs not only have antibacterial effects, but also enhance the effect of OMP by inhibiting its metabolism by CYP2C19. These results indicate that drug-drug interactions of co-administered drugs can cause complex effects, providing a basis for OMP dose adjustment when used in combination therapy for H. pylori eradication.


Assuntos
Antibacterianos/farmacologia , Citocromo P-450 CYP2C19/metabolismo , Infecções por Helicobacter/tratamento farmacológico , Helicobacter pylori/efeitos dos fármacos , Omeprazol/farmacologia , Amoxicilina/química , Amoxicilina/farmacologia , Antibacterianos/química , Antibacterianos/metabolismo , Cromatografia Líquida de Alta Pressão , Claritromicina/química , Claritromicina/farmacologia , Citocromo P-450 CYP2C19/química , Combinação de Medicamentos , Humanos , Metronidazol/química , Metronidazol/farmacologia , Testes de Sensibilidade Microbiana , Estrutura Molecular , Omeprazol/antagonistas & inibidores , Omeprazol/metabolismo , Tinidazol/química , Tinidazol/farmacologia
15.
Chem Pharm Bull (Tokyo) ; 67(8): 884-887, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31366837

RESUMO

We developed a simple and sensitive HPLC method for the determination of selenocyanate (SeCN-). The König reaction, which is generally used for the determination of cyanide and thiocyanate, was applied for the post-column detection, and using barbituric acid as a fluorogenic reagent made it possible to detect SeCN- with high sensitivity. The limits of detection (LOD) and quantification (LOQ) were 73.5 fmol and 245.1 fmol, respectively. Subsequently, the amounts of SeCN- in human blood and in cultured cell samples were analyzed, and no SeCN- was detected in human whole blood. Interestingly, we have found that some of the spiked SeCN- decomposed to cyanide in human whole blood. Ascorbic acid suppressed the decomposition of SeCN- to cyanide by reducing the ferric ion, which is typically involved in SeCN- decomposition. Then, SeCN- was detected in cultured HEK293 cells exposed to selenite. The established HPLC method with fluorescence detection of SeCN- is useful for investigating small amounts of SeCN- in biological samples.


Assuntos
Cianatos/sangue , Fluorescência , Compostos de Selênio/sangue , Células Cultivadas , Cromatografia Líquida de Alta Pressão/instrumentação , Células HEK293 , Humanos
16.
J Agric Food Chem ; 67(33): 9362-9370, 2019 Aug 21.
Artigo em Inglês | MEDLINE | ID: mdl-31368700

RESUMO

This manuscript presents an effective and robust method for simultaneous stereoselective determination of two pyrethroid insecticides, tetramethrin and α-cypermethrin in different food products by high-performance liquid chromatography. Enantioseparation was carried out using reversed-phase chromatography, and the influences of four polysaccharide-based chiral columns, mobile phase composition, and column temperature on retention were fully investigated. Satisfactory separation was obtained on Chiralpak IG column using acetonitrile-water (75:25, v/v) under isocratic conditions. To extract and purify the target analytes from food matrices, matrix solid-phase dispersion was employed with C18 as dispersant and primary secondary amine as well as graphitized carbon black as cleanup sorbents. Response surface method based on Box-Behnken design was implemented to assist optimization of the extraction variables. Then, method validation was done in real samples including specificity, linearity, sensitivity, trueness, precision, as well as stability, and its analytical performance fulfills the criteria recommended by the European Union SANTE/11945/2015, demonstrating its applicability in studying the stereochemistry of chiral tetramethrin and α-cypermethrin in food products.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Grão Comestível/química , Frutas/química , Inseticidas/química , Piretrinas/química , Verduras/química , Cromatografia de Fase Reversa/métodos , Contaminação de Alimentos/análise , Inseticidas/isolamento & purificação , Piretrinas/isolamento & purificação , Extração em Fase Sólida , Estereoisomerismo
17.
Shokuhin Eiseigaku Zasshi ; 60(3): 61-67, 2019.
Artigo em Japonês | MEDLINE | ID: mdl-31391412

RESUMO

A method was developed for the determination of nonvolatile amines, such as histamine, tyramine, putrescine, and cadaverine, in foods. These nonvolatile amines were extracted from a sample with 5% trichloroacetic acid, and the extract was purified using an InertSep MC-1 cartridge column. The four amines were derivatized with fluorescamine, determined by HPLC with a fluorescence detector, and confirmed by LC-MS/MS. The average recoveries (n=5) and the relative standard deviations from 11 foods (pacific saury, dried mackerel, canned mackerel in brine, canned tuna in oil, fish sauce, surimi, rice-koji miso, soy sauce, gouda cheese, red wine, and beer) spiked at 100 mg/kg were 81-100% and 0.4-3.1%, respectively.


Assuntos
Aminas/análise , Fluorescamina , Análise de Alimentos/métodos , Animais , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas em Tandem
18.
Anticancer Res ; 39(8): 4043-4053, 2019 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-31366486

RESUMO

BACKGROUND/AIM: Triple-negative breast cancer (TNBC) is the most aggressive subtype, predominant in African American women. In this study, the antioxidant/anticancer activity of muscadine grape extracts and the role of their phenolic and flavonoid contents in exerting these properties were investigated in TNBC cells. MATERIALS AND METHODS: Berry extracts from muscadine genotypes were investigated for total phenolic content (TPC), total flavonoid content (TFC), antioxidant capacity, and anticancer effects using breast cancer cell lines, representing Caucasians and African Americans. RESULTS: The antioxidant activity was associated with high TPC content. Extracts showed cytotoxicity up to 78.6% in Caucasians and 90.7% in African American cells, with an association with high antioxidant capacity. There was a strong correlation between TPC and anticancer/antioxidant activities. CONCLUSION: The anticancer and antioxidant effects of muscadine grapes are attributed to the TPC of extracts, which showed a stronger positive correlation with growth inhibition of African American breast cancer cells compared to Caucasians.


Assuntos
Antineoplásicos Fitogênicos/farmacologia , Extratos Vegetais/farmacologia , Neoplasias de Mama Triplo Negativas/tratamento farmacológico , Vitis/química , Afro-Americanos/genética , Antineoplásicos Fitogênicos/química , Antioxidantes/química , Antioxidantes/farmacologia , Linhagem Celular Tumoral , Cromatografia Líquida de Alta Pressão , Feminino , Flavonoides/química , Flavonoides/farmacologia , Frutas/química , Humanos , Células MCF-7 , Fenóis/química , Fenóis/farmacologia , Extratos Vegetais/química , Neoplasias de Mama Triplo Negativas/genética , Neoplasias de Mama Triplo Negativas/patologia
19.
An Acad Bras Cienc ; 91(3): e20180621, 2019 Aug 12.
Artigo em Inglês | MEDLINE | ID: mdl-31411258

RESUMO

Aristolochia triangularis Cham., is one of the most frequently used medicinal plant in Southern Brazil. Preparations containing the leaves and/or stems are traditionally used as anti-inflammatory, diuretic, as well as antidote against snakebites. This study screened A. triangularis extracts, fractions and isolated compounds for different bioactivities. A weak antiproliferative activity against human lung cancer cell line (A549) was observed only for chloroform fraction obtained from stems (CFstems - CC50: 2.93 µg/mL). Also, a moderate antimicrobial activity against Staphylococcus aureus was detected just for chloroform fraction obtained from leaves (CFleaves -13-16 mm inhibition zone). Additionally, two semi-purified fractions (CFstems-4 and CFleaves-4) selectively inhibited HSV-1 replication (IC50 values of 0.40 and 2.61 µg/mL, respectively), while only CFleaves showed promising results against Leishmania amazonensis. Fractionation of extracts resulted in the isolation of one neolignan (-) cubebin and one lignan (+) galbacin. However, these compounds are not responsible for the in vitro bioactivities herein detected. The presence of aristolochic acid I and aristolochic acid II in the crude ethanol extract of stems (CEEstems) and leaves (CEEleaves) was also investigated. The HPLC analysis of these extracts did not display any peak with retention time or UV spectra comparable to aristolochic acids I and II.


Assuntos
Aristolochia/química , Compostos Fitoquímicos/química , Antibacterianos/farmacologia , Antifúngicos/farmacologia , Antiprotozoários/farmacologia , Antivirais/farmacologia , Ácidos Aristolóquicos/química , Brasil , Fracionamento Químico , Cromatografia Líquida de Alta Pressão/métodos , Humanos , Compostos Fitoquímicos/farmacologia , Extratos Vegetais/farmacologia
20.
J Cosmet Sci ; 70(4): 167-180, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31441771

RESUMO

A worldwide outbreak of skin cancer, related to ultraviolet (UV) radiations, was reported. Therefore, primary prevention programs were initiated. Application of sunscreens is one of the most efficient ways of protection; however, their efficiency and safety have remained a challenging issue. So, it seems necessary to consider the potential side effects for limiting the use and amount of sunscreens. In this study, an high performance liquid chromatography (HPLC) system equipped with a UV-visible detector has been used. For separation, an Agilent C18 column was used (Agilent Technologies, Santa Clara, CA). This method was applied for quantitative determination of nine UV filters in commercial sunscreen products which were widely used in Iran. Fifty samples of Iranian and imported sunscreen products were analyzed. The detection limit was determined to be 0.439-1.481 µg/ml, and the quantization limit was determined to be 1.330-4.490 µg/ml. Also, in this study, chemometric methods were used to investigate the differences between Iranian and other countries' sunscreen brands. It was observed that despite the amount of UV filters in Iranian sunscreens, which was in the allowed range, there were some differences between Iranian and other countries' sunscreens. The proposed HPLC method allows efficient and simultaneous analysis of UV filters and is suitable as a quality control assay for commercial sunscreen products.


Assuntos
Protetores Solares/química , Raios Ultravioleta , Cromatografia Líquida de Alta Pressão , Irã (Geográfico) , Limite de Detecção
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