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1.
Biol Trace Elem Res ; 2019 Nov 09.
Artigo em Inglês | MEDLINE | ID: mdl-31707637

RESUMO

For the first time, bioavailability, pharmacokinetics, and biotransformation of selenium-enriched yeast (SeY) and sodium selenite (Na2SeO3) in rats were systemically compared by analyzing free selenomethionine (SeMet), total SeMet, and selenium (Se). After SeY and Na2SeO3 were orally administered to rats at a dose of 100 µg Se/kg, plasma free SeMet, total SeMet, and Se at various time points were determined by ultra-performance liquid chromatography-tandem mass spectrometry. Based on Se and total SeMet, the relative bioavailability values of SeY compared with Na2SeO3 were 144% and 272%, respectively. For the rats treated with SeY, 0.73-2.68% of total Se was biotransformed to free SeMet, 14.3-20.4% to SeMet-proteins and albumin-bound SeMet, and 75.9-82.3% to selenoproteins in plasma. SeY had higher bioavailability than Na2SeO3 based on Se and total SeMet levels. Plasma SeMet was the optimal biomarker of SeY status in vivo.

2.
Asia Pac J Clin Nutr ; 28(2): 341-346, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-31192563

RESUMO

BACKGROUND AND OBJECTIVES: A reliable biomarker for optimal selenium (Se) intake in lactating women is not currently available. METHODS AND STUDY DESIGN: Daily dietary Se intake in lactating women was calculated from a 24-hour meal record survey for over 3 days. Se levels in plasma and breast milk were measured through inductively coupled plasma mass spectrometry. Plasma selenoprotein P 1 levels and glutathione peroxidase 3 activity were measured using an enzyme-linked immunosorbent assay. Ultra-performance liquid chromatography-tandem mass spectrometry was used to analyze proteinaceous Se species in enzymatically digested breast milk. RESULTS: Dietary Se intakes of lactating women from Liangshan, Beijing, and Enshi were 41.6±21.2 ng/d, 51.1±22.6 ng/d, and 615±178 ng/d, respectively (p<0.05). The Se levels in the blood and breast milk were significantly associated with the dietary Se intake (p<0.05). The proteinaceous Se species in breast milk were SeMet and SeCys2. The levels of SeMet in the lactating women from Liangshan, Beijing, and Enshi were 3.31±2.44 ng Se/mL, 7.34±3.70 ng Se/mL, and 8.99±9.64 ng Se/mL, while that of SeCys2 were 13.7±12.0 ng Se/mL, 35.6±20.9 ng Se/mL, and 57.4±13.2 ng Se/mL, respectively. Notably, the concentration of SeCys2, the metabolite of unstable SeCys, reached a saturation platform, whereas no similar phenomenon were found for the total Se SeMet from Secontaining proteins. CONCLUSIONS: SeCys2 in breast milk is a potential biomarker for determining the optimal Se intake in lactating women.

3.
Food Chem ; 293: 169-177, 2019 Sep 30.
Artigo em Inglês | MEDLINE | ID: mdl-31151598

RESUMO

Antioxidant molecules in honey contributed to various biological effects, but antioxidant components markers in honey are required to be investigated further. Phenolic compounds, flavonoids and free amino acids were analyzed using UPLC-MS/MS and HPLC-FLD from 39 honey samples, in which fennel honey was firstly investigated. Based on the quantitative composition-activity relationship, the cellular antioxidant activity (CAA) assay of various honeys is closely related with the interaction of some phenolic compounds (isoferulic acid, 3,4-dihydroxy benzoic acid, 4-hydroxy benzoic acid, chlorogenic acid, caffeic acid, gallic acid, cryptochlorogenic acid, p-coumaric acid, salicylic acid), flavonoids (isosakuranetin, sakuranetin, pinocembrin, vitexin, taxifolin, galangin, luteolin, chrysin) and free amino acids (Tyr, Gly, Ile, Glu, Val, Phe, Leu, Asp, His, Pro, Ala). The results would be beneficial for the understanding of the nutritional values, exploitation and utilization of honeys with different floral origins, further contributable to the market development and consumption choice of honey.


Assuntos
Antioxidantes/análise , Mel/análise , Aminoácidos/análise , Aminoácidos/química , Antioxidantes/química , Cromatografia Líquida de Alta Pressão/métodos , Flavonoides/análise , Flavonoides/química , Análise dos Mínimos Quadrados , Fenóis/análise , Fenóis/química , Espectrometria de Massas em Tandem
4.
Biol Trace Elem Res ; 2018 Aug 01.
Artigo em Inglês | MEDLINE | ID: mdl-30069692

RESUMO

Zinc (Zn) highly concentrates in the brain and plays a key role in memory formation and learning processes. Zn deficiency results in cognitive impairments, memory deficits, alterations of neuropsychological behavior, and motor development. Although Zn-enriched yeast (ZnY) is widely used for dietary fortification and supplementation of Zn, the effect of ZnY on cognition still remains unclear. The purpose of the study was to investigate the effect of ZnY on behavior in Zn-deficient and Zn-sufficient rats. Three-week-old rats were fed low Zn diets for 145 days to establish Zn-deficient rats. ZnY was orally administered to Zn-deficient rats at three dose levels of 1, 2, and 4 mg Zn/kg/day for 55 days. Rat appearance, body weight, plasma and brain Zn, Morris water maze test, and step-through passive avoidance test were observed. Compared to Zn-sufficient rats, body weight gain, plasma zinc level, resident time, and step-through time in Zn-deficient rats were significantly lower. Zn deficiency impaired functions of learning and memory, while ZnY as a plausible therapeutic intervention alleviated the cognitive impairments caused by Zn deficiency.

5.
Molecules ; 23(5)2018 May 08.
Artigo em Inglês | MEDLINE | ID: mdl-29738446

RESUMO

Phenolics and flavonoids in honey are considered as the main phytonutrients which not only act as natural antioxidants, but can also be used as floral markers for honey identification. In this study, the chemical profiles of phenolics and flavonoids, antioxidant competences including total phenolic content, DPPH and ABTS assays and discrimination using chemometric analysis of various Chinese monofloral honeys from six botanical origins (acacia, Vitex, linden, rapeseed, Astragalus and Codonopsis) were examined. A reproducible and sensitive ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was optimized and validated for the simultaneous determination of 38 phenolics, flavonoids and abscisic acid in honey. Formononetin, ononin, calycosin and calycosin-7-O-β-d-glucoside were identified and quantified in honeys for the first time. Principal component analysis (PCA) showed obvious differences among the honey samples in three-dimensional space accounting for 72.63% of the total variance. Hierarchical cluster analysis (HCA) also revealed that the botanical origins of honey samples correlated with their phenolic and flavonoid contents. Partial least squares-discriminant analysis (PLS-DA) classification was performed to derive a model with high prediction ability. Orthogonal partial least squares-discriminant analysis (OPLS-DA) model was employed to identify markers specific to a particular honey type. The results indicated that Chinese honeys contained various and discriminative phenolics and flavonoids, as well as antioxidant competence from different botanical origins, which was an alternative approach to honey identification and nutritional evaluation.


Assuntos
Antioxidantes/química , Flavonoides/química , Mel/análise , Fenóis/química , Acacia/química , Astrágalo (Planta)/química , Brassica rapa/química , Cromatografia Líquida de Alta Pressão , Análise Discriminante , Flavonoides/isolamento & purificação , Flores/química , Fenóis/isolamento & purificação , Análise de Componente Principal , Espectrometria de Massas em Tandem , Tilia/química , Vitex/química
6.
Asia Pac J Clin Nutr ; 27(2): 284-292, 2018.
Artigo em Inglês | MEDLINE | ID: mdl-29384312

RESUMO

Formula-based animal milk is an alternative source of infant nutrition in many cases when breastfeeding is unacceptable or inaccessible; however, these replacements often have low selenium levels. The composition of infant formula milk should be as close as possible to that of human breast milk, both in content and chemical speciation. Selenium is an essential trace element for infants. Generally, human breast milk is the ideal food to ensure adequate infant Se intake. However, to date, sodium selenite or sodium selenate has been used as selenium supplementation in infant formula milk in most countries. This inorganic Se, which is not a natural component of food, may not be the optimal speciation for Se supplementation in infant formula milk. Advances in speciation in foods, especially in animal milk, suggest that future proposals for selenium speciation in human breast milk can lead to discussions regarding the most favorable methods of selenium supplementation in infant formula milk.

7.
Mol Nutr Food Res ; 62(7): e1700981, 2018 04.
Artigo em Inglês | MEDLINE | ID: mdl-29457347

RESUMO

SCOPE: The oral absorption, distribution, excretion, and bioavailability of zinc sulfate (ZnS), zinc gluconate (ZnG), and zinc-enriched yeast (ZnY) in rats are fully and systemically compared for the first time. METHODS AND RESULTS: After zinc compounds were orally administered to rats at a single dose of 4 mg Zn kg-1 , blood, tissues, urine, and feces at different time points were collected for the quantification of zinc concentration. Blood was also harvested for the zinc assay in the multiple-dose administration. Plasma zinc levels among three zinc compounds showed no difference, and zinc was widely distributed in various tissues with the level sequence of bone > liver > pancreas > testes. The net Zn balance was 2.993, 5.125, and 7.482% for ZnS, ZnG, and ZnY, respectively. CONCLUSION: ZnS, ZnG, and ZnY show equivalent bioavailability based on plasma and tissues zinc levels, although ZnY was statistically more absorbed and retained than ZnS and ZnG based on the excretion amount.

8.
Food Chem ; 241: 1-6, 2018 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-28958505

RESUMO

The in vivo determination of selenomethionine (SeMet) converted from selenium-enriched yeast (SeY) rather than the determination of in vitro hydrolyzed SeMet is a better parameter for the evaluation of SeY quality. A UPLC-MS/MS method was developed for the quantification of SeMet in rat plasma and the oral bioavailability of SeMet converted from SeY in rats. After a simple extraction with perchloric acid, SeMet and the internal standard methylselenocysteine (MSC) were separated on a C18 column with isocratic elution of water:acetonitrile:formic acid (99:1:0.1, v/v/v) and detected in the multiple reaction monitoring mode. The method was accurate (92.6-104.3%) and precise (1.8-11.0%), and the recovery was 79.4-95.4%. It was successfully applied to pharmacokinetic and bioavailability studies of SeY in rats following the intravenous administration of SeMet and intragastric administration of SeY. SeMet in vivo, converted from SeY, is reported for the first time, and the results suggested that the SeY bioavailability in rats is 87%.


Assuntos
Selênio/química , Selenometionina/química , Administração Oral , Animais , Ratos , Ratos Sprague-Dawley , Espectrometria de Massas em Tandem , Fermento Seco
9.
Drug Test Anal ; 9(10): 1604-1610, 2017 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-28303675

RESUMO

Icaritin (ICT) displays numerous pharmacological activities for the treatment of various cancers, osteoporosis, inflammation, and angiocardiopathy. The absorption, distribution, metabolism, and excretion of ICT still remain unknown. ICT was administered to rats at 2 mg/kg for intravenous injection or 40 mg/kg for oral route. Major metabolite of ICT was identified using quadrupole time-of-flight (Q-TOF), and ICT and its major metabolite were quantified in plasma, tissues, urine, faeces, and bile by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). A total of 24 metabolites of ICT in plasma were identified and mono C-7 glucuronide glucuronidated icaritin (GICT) was the major metabolite of ICT after oral administration. The absolute bioavailability of ICT was 4.33% although ICT was rapidly absorbed into the blood. For oral administration, concentrations of GICT at various time points was 6.38-8.81-fold higher than those of ICT, and the area under the curve (AUC) of GICT was about 8-fold higher than that of ICT, while AUC values of ICT and GICT were almost equal for intravenous injection. Approximately 65.7% ICT and 42.7% GICT were distributed in liver and kidney, respectively. Unabsorbed ICT was mainly excreted as the parent form in faeces with at least 60% of administered dose during 24 h, whereas absorbed ICT was predominantly excreted as GICT from urine with 2.74% of administered dose accounting for 63.28% of absorbed drug. ICT was rapidly absorbed into the blood although a large amount of ICT remained unabsorbed, and then rapidly and mainly metabolized to GICT. ICT mainly distributed in liver, while GICT predominantly distributed in kidney. Absorbed ICT and GICT were predominantly excreted via urine, and unabsorbed ICT was mainly excreted as the parent form in faeces. Copyright © 2017 John Wiley & Sons, Ltd.


Assuntos
Anti-Inflamatórios/farmacocinética , Antineoplásicos/farmacocinética , Flavonoides/farmacocinética , Administração Oral , Animais , Anti-Inflamatórios/administração & dosagem , Anti-Inflamatórios/sangue , Anti-Inflamatórios/metabolismo , Antineoplásicos/administração & dosagem , Antineoplásicos/sangue , Antineoplásicos/metabolismo , Cromatografia Líquida de Alta Pressão/métodos , Flavonoides/administração & dosagem , Flavonoides/sangue , Flavonoides/metabolismo , Masculino , Ratos , Ratos Sprague-Dawley , Espectrometria de Massas em Tandem/métodos , Distribuição Tecidual
10.
Anal Sci ; 32(6): 631-7, 2016.
Artigo em Inglês | MEDLINE | ID: mdl-27302583

RESUMO

Icaritin (ICT), a major component in herb Epimedium brevicornum Maxim., shows beneficial effects for the treatment of osteoporosis and various cancers, and is predominantly metabolized to glucuronidated icaritin (GICT). Although clinical trials of ICT have exhibited good safety and tolerance, the dynamic bioditributions of ICT and GICT have not been reported. In the present study, the chemical structure of GICT was firstly reported, and a reliable ultra-high performance liquid chromatography-tandem mass spectrometry method (UHPLC-MS/MS) was firstly established for the simultaneous quantifications of ICT and GICT in rat tissues. The dynamic distribution of ICT and GICT in rat tissues and their pharmacokinetic parameters have been reported for the first time. ICT, GICT and the internal standard coumestrol were separated on a C18 column with a gradient mobile phase of acetonitrile and water containing ammonium formate and formic acid at a flow rate of 0.3 mL min(-1). The analytes were quantified by a triple quadrupole tandem mass spectrometer in the negative ionization mode. The lower limit of quantification values for ICT and GICT were 0.2 and 2 ng mL(-1), respectively. Good selectivity, linearity, accuracy, precision and recovery were achieved, and no significant matrix effect was observed. The UHPLC-MS/MS was firstly applied to a dynamic biodistribution study of ICT and GICT in rats, following an intraperitoneal administration of ICT at a dose of 10 mg kg(-1).


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Flavonoides/farmacocinética , Desintoxicação Metabólica Fase II , Espectrometria de Massas em Tandem/métodos , Animais , Flavonoides/metabolismo , Glucuronídeos/metabolismo , Ratos , Ratos Sprague-Dawley , Reprodutibilidade dos Testes , Distribuição Tecidual
11.
Artigo em Inglês | MEDLINE | ID: mdl-25531867

RESUMO

Icaritin (ICT), a bioactive metabolite of prenylflavonoids from genus Epimedium, has displayed potential benefits for the treatment of osteoporosis, prostate cancer, liver cancer, renal cancer and breast cancer. To investigate the quantity of ICT in bones in vivo, a simple and sensitive ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed. After a rapid one-step liquid-liquid extraction using ethyl acetate with recovery more than 87.2% at four levels (0.1, 0.2, 8 and 15 ng/mL), ICT and internal standard coumestrol were analyzed on a C18 column using a gradient elution of acetonitrile and water containing ammonium formate and formic acid at a flow rate of 0.3 mL/min. Quantification was performed using selected reaction monitoring mode to monitor precursor-product ion transitions of m/z 367.1→297.1 for ICT and of 267.0→211.1 for coumestrol in the negative ionization mode. A calibration curve with good linearity (r>0.99) within the concentration range of 0.1-20 ng/mL for ICT was obtained with the lower limit of quantification of 0.1 ng/mL. Matrix effect did not interfere with ICT analysis and ICT was stable under three freeze-thaw cycles, short-term temperature, post-preparative and long-term temperature conditions. The method was successfully applied to a dynamic distribution of ICT in mouse bone after a single intraperitoneal administration to ICT to mice.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Flavonoides/análise , Coluna Vertebral/química , Espectrometria de Massas em Tandem/métodos , Animais , Flavonoides/administração & dosagem , Flavonoides/farmacocinética , Injeções Intraperitoneais , Modelos Lineares , Camundongos , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
13.
J Ethnopharmacol ; 155(2): 1382-7, 2014 Sep 11.
Artigo em Inglês | MEDLINE | ID: mdl-25086407

RESUMO

ETHNOPHARMACOLOGICAL RELEVANCE: Icaritin (ICT) is a major bioactive prenylflavonoid derivative contained in the Epimedium which is a widely used herbal medicine for the treatment of infertility, impotence, cardiovascular and skeletal diseases listed in the Chinese Pharmacopoeia. The aim of this study is to investigate the tissue distribution of ICT in rats by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) MATERIALS AND METHODS: ICT was intraperitoneally administrated to rats for 7 consecutive days at dose levels of 20, 40 and 60 mg/kg/day, respectively. Various tissue homogenates were pretreated by protein precipitation with acetonitrile. ICT and internal standard coumestrol were separated on a BEH C18 column with a gradient mobile phase and detected using precursor-product ion transitions of m/z 367.1→297.1 for ICT and 267.0→211.1 for coumestrol at the negative ionization mode, respectively. RESULTS: ICT was widely distributed in rat's various tissues and its concentrations in tissues increased with elevated doses. A sensitive and reliable UPLC-MS/MS method was firstly established to quantify ICT in rat tissues. The lower limit of quantification was 0.5 ng/mL based on 100 µL of tissue homogenates. The intra- and inter-day accuracy at all levels fell in the ranges of 90.8-103.4% and 91.6-100.3%, and the intra- and inter-day precision (RSD) were in the ranges of 2.9-10.5% and 2.6-9.1%, respectively. CONCLUSIONS: The UPLC-MS/MS showed good accuracy, precision and recovery and was suitable for the quantification of ICT in rat tissues. Wide distribution of ICT could helpfully elucidate systemic effects and various functions of ICT.


Assuntos
Cromatografia Líquida , Flavonoides/farmacocinética , Espectrometria de Massas em Tandem , Animais , Feminino , Flavonoides/administração & dosagem , Humanos , Injeções Intraperitoneais , Limite de Detecção , Modelos Lineares , Variações Dependentes do Observador , Ratos Sprague-Dawley , Reprodutibilidade dos Testes , Distribuição Tecidual
14.
J Anal Methods Chem ; 2014: 975820, 2014.
Artigo em Inglês | MEDLINE | ID: mdl-24701366

RESUMO

A rapid, accurate, and high performance method of high resolution sector field inductively coupled plasma mass spectrometry (HR-ICP-MS) combined with a small-size sample (0.1 mL) preparation was established. The method was validated and applied for the determination of 16 selected plasma trace elements (Fe, Cu, Zn, Rb, B, Al, Se, Sr, V, Cr, Mn, Co, As, Mo, Cd, and Pb). The linear working ranges were over three intervals, 0-1 µ g/L, 0-10 µ g/L and 0-100 µ g/L. Correlation coefficients (R (2)) ranged from 0.9957 to 0.9999 and the limits of quantification (LOQ) ranged from 0.02 µ g/L (Rb) to 1.89 µ g/L (Se). The trueness (or recovery) spanned from 89.82% (Al) to 119.15% (Se) and precision expressed by the relative standard deviation (RSD %) for intra-day ranging from 1.1% (Zn) to 9.0% (Se), while ranged from 3.7% (Fe) to 12.7% (Al) for interday. A total of 440 plasma samples were collected from Chinese National Nutrition and Health Survey Project 2002 (CNNHS 2002), which represented the status of plasma trace elements for the children aged 3-12 years from China economical developed rural areas. The concentrations of 16 trace elements were summarized and compared by age groups and gender, which can be used as one of the basic components for the formulation of the baseline reference values of trace elements for the children in 2002.

15.
Biomed Chromatogr ; 28(3): 433-8, 2014 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-24115152

RESUMO

Psoralea Corylifolia L. is a traditional Chinese medicine with many beneficial effects in medical therapies. Bakuchiol was the main active ingredient of Psoralea Corylifolia L., used for the treatment of various diseases and also as a natural food additive. A specific and reliable ultra-high performance liquid chromatography-tandem mass spectrometry has been developed and fully validated for the quantification of bakuchiol in rat plasma. Chromatographic separation of bakuchiol and an internal standard, daidzein, was achieved on a Hypersil Gold C18 column with gradient elution that consisted of methanol and water at a flow rate of 0.2 mL/min. The compounds were detected at negative ionization mode using mass transition m/z 255.2 → 172.0 and 252.9 → 132.0 for bakuchiol and daidzein, respectively. Good linearity was obtained over the range of 2-1000 ng/mL and the lower limit of quantification was 2 ng/mL. The intra- and inter-day accuracies ranged from 91.1 to 105.7% and precisions (relative standard deviations) were within 9.3%. Bakuchiol was found to be stable under three freeze-thaw cycles, short-term temperature, post-preparative and long-term temperature conditions. The method was applied to a pharmacokinetic study of bakuchiol intravenously administered to rats at a dose of 5 mg/kg.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Fenóis/sangue , Fenóis/farmacocinética , Espectrometria de Massas em Tandem/métodos , Animais , Estabilidade de Medicamentos , Modelos Lineares , Masculino , Fenóis/química , Ratos , Ratos Sprague-Dawley , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
17.
Artigo em Inglês | MEDLINE | ID: mdl-23010480

RESUMO

A sensitive and reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed and validated for the determination of andrographolide sodium bisulphite (ASB) in dog plasma using dehydroandrographolide (DAG) as an internal standard. Chromatographic separation was achieved on a Hypersil Gold C(18) column (50 mm × 2.1 mm, 1.9 µm) with gradient elution that consisted of methanol and water at a flow rate of 0.2 mL/min. Quantification was done using selected reaction monitoring (SRM) mode to monitor precursor-product ion transitions of m/z 413.2→287.2 for ASB and 331.2→303.3 for DAG at negative ionization mode. Good linearity was obtained over the range of 10-1000 ng/mL and the correlation coefficient was better than 0.99. The intra- and inter-day accuracies ranged from 97.2% to 107.8% and precisions (RSD) were within 13.9%. ASB was found stable under three freeze-thaw cycles, short-term temperature, post-preparative and long-term temperature conditions. The method was successfully applied to a pharmacokinetic study of ASB intravenously administered to Beagle dogs.


Assuntos
Cromatografia Líquida/métodos , Diterpenos/sangue , Sulfitos/sangue , Espectrometria de Massas em Tandem/métodos , Animais , Diterpenos/química , Diterpenos/farmacocinética , Cães , Estabilidade de Medicamentos , Modelos Lineares , Masculino , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Sulfitos/química , Sulfitos/farmacocinética
18.
Artigo em Inglês | MEDLINE | ID: mdl-22130502

RESUMO

A liquid chromatography-tandem mass spectrometry method for the determination of andrographolide sodium bisulphite (ASB) in rat urine was established and validated. To our knowledge, the analytical method is the first developed assay for the determination of ASB in urine samples. Dehydroandrographolide (DAG) was used as an internal standard. ASB and DAG were separated on a C(18) column and detected at negative ion mode using the mass transitions of m/z 413.2→287.2 and m/z 331.2→303.3, respectively. Good linearity was obtained over the range of 50-5000 ng/mL and the correlation coefficient was better than 0.99. The intra- and inter-day accuracy at all levels fell in the ranges of 85.8-101.4% and 87.9-97.5%, and the intra- and inter-day precision (RSD) were in the ranges of 4.3-11.2% and 8.4-13.3%, respectively. The recovery ranged from 96.1% to 98.3% and the matrix effects from 96.2% to 98.1%. Good stability was found under tested conditions. The method was successfully applied to a urinary excretion study of ASB in rats following intravenous administration of 80 mg/kg ASB.


Assuntos
Cromatografia Líquida/métodos , Diterpenos/urina , Sulfitos/urina , Espectrometria de Massas em Tandem/métodos , Animais , Diterpenos/administração & dosagem , Diterpenos/química , Diterpenos/farmacocinética , Estabilidade de Medicamentos , Feminino , Injeções Intravenosas , Modelos Lineares , Masculino , Ratos , Ratos Sprague-Dawley , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Sulfitos/química , Sulfitos/farmacocinética
19.
J Chromatogr B Analyt Technol Biomed Life Sci ; 879(31): 3763-6, 2011 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-22055830

RESUMO

UP302 is a novel natural antioxidant isolated from Dianella ensifolia (Liliaceae). In the investigation, a specific and sensitive ultra-high performance liquid chromatography-tandem mass spectrometry for quantitative determination of UP302 in rat plasma was developed and validated. UP302 and the internal standard daidzein were extracted from 100 µL aliquots of rat plasma using methanol. Detection of UP302 and IS was done by tandem mass spectrometry, operating in negative ion and selected reaction monitoring acquisition mode. The precursor-product ion transitions monitored for UP302 and daidzein were m/z 301.1→135.2 and 252.9→132.0, respectively. The linearity of the method was observed within the concentration range of 5-2000 ng/mL. Intra- and inter-day assay variations were less than 15%, and the accuracy values were between 99.2% and 107.3%. The method was successfully applied to stability investigation of UP302 incubated in rat plasma at 37°C and measurement of UP302 in plasma after intravenous administration of UP302 to rats at a single dose of 5 mg/kg. Incubation stability revealed that within first one hour, UP302 was rapidly declined approximately 35% and remained stable after 4 h. Pharmacokinetic values of half-life, volume of distribution, systemic clearance and mean residence time were 0.87 ± 0.58 h, 6.90 ± 3.35 L/kg, 5.89 ± 1.21 L/h kg and 0.34 ± 0.13 h, respectively.


Assuntos
Antioxidantes/análise , Cromatografia Líquida de Alta Pressão/métodos , Fenóis/sangue , Propano/análogos & derivados , Espectrometria de Massas em Tandem/métodos , Animais , Antioxidantes/administração & dosagem , Antioxidantes/farmacocinética , Estabilidade de Medicamentos , Liliaceae/química , Limite de Detecção , Masculino , Fenóis/administração & dosagem , Fenóis/farmacocinética , Propano/administração & dosagem , Propano/sangue , Propano/farmacocinética , Ratos , Ratos Sprague-Dawley , Reprodutibilidade dos Testes , Temperatura Ambiente
20.
J Chromatogr B Analyt Technol Biomed Life Sci ; 879(7-8): 548-52, 2011 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-21296037

RESUMO

A sensitive and selective liquid chromatographic-tandem mass spectrometric method was developed for quantification of triamcinolone acetonide (TA) in rabbit ocular tissues. After a simple liquid-liquid extraction using tert-butyl methyl ether, TA and internal standard methylprednisolone were separated on a C18 column with a mobile phase of acetonitrile:water:formic acid (60:40:0.1, v/v/v) and quantified by the use of selected reaction monitoring mode with a total run time of 4 min. The method was validated in tissue homogenates with a daily working range of 1-1000 ng/mL with correlation coefficient of more than 0.99 and a sensitivity of 1 ng/mL as lower limit of quantification, respectively. The mean intra-day and inter-day precisions were less than 10% and accuracy values were higher than 90%. This method was fully validated for the accuracy, precision and stability studies. The method proved to be accurate and specific, and was applied to an in vivo biodistribution study of TA after intravitreal injection to rabbits. Values of mean residence time in vitreous humor, crystalline lens and aqueous humor were 27.7, 35.8 and 20.0 days, respectively.


Assuntos
Humor Aquoso/química , Cromatografia Líquida/métodos , Cristalino/química , Espectrometria de Massas em Tandem/métodos , Triancinolona Acetonida/análise , Corpo Vítreo/química , Animais , Humor Aquoso/metabolismo , Estabilidade de Medicamentos , Injeções Intravítreas , Cristalino/metabolismo , Masculino , Coelhos , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Distribuição Tecidual , Triancinolona Acetonida/administração & dosagem , Triancinolona Acetonida/farmacocinética , Corpo Vítreo/metabolismo
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