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1.
A highly sensitive and specific atmospheric pressure chemical ionization liquid chromatography-tandem mass spectrometry method was developed for serum pharmacokinetic studies of puerarin in rats. Chromatography was carried out on a reversed-phase Phenomenex Synergi 4 microm Fusion-RP80 column (150 x 2.0 mm i.d.) using a mobile phase consisting of acetonitrile-water (10:90, v/v) in 10 mm NH(4)OAc with a flow rate of 0.2 mL/min. Puerarin was analyzed in the multiple reaction monitoring mode with a precursor/product ion transition of m/z 415/267. The method was demonstrated to be specific and sensitive, and a linear response was observed over a range of 2-5000 ng/mL in rat serum. The validated method was successfully applied to the characterization of the pharmacokinetics of puerarin in rat serum after oral administration to spontaneously hypertensive rats. The blood concentration-time profile of puerarin showed a rapid initial increase, reaching a maximum and then declining within 1 h. Puerarin could not be detected after 24 h. The main pharmacokinetic parameters for puerarin after oral administration were as follows: C(max) (3.54 +/- 2.03 mg/L), T(max) (0.68 +/- 0.37 h), AUC(0-t) (7.29 +/- 3.79 mg h/L), AUC(0-infinity) (9.17 +/- 4.87 mg h/L), T(1/2) (1.7 +/- 0.6 h), CL/F (7.24 +/- 4.27 L/h/kg) and V/F (17.88 +/- 13.55 L/h/kg).  相似文献   

2.
杨蕾  唐中华  祖元刚 《色谱》2007,25(4):550-552
运用高效液相色谱(HPLC)梯度洗脱同时测定了长春花中的文多灵、长春质碱和脱水长春碱等3种生物碱。色谱柱为Waters 5C18-MS-Ⅱ(4.6 mm×250 mm),流动相为甲醇-1%二乙胺(磷酸调pH至7.3)系统,梯度洗脱,检测波长220 nm,柱温25 ℃。实验结果表明,文多灵、长春质碱和脱水长春碱等3种生物碱分别在0.03~1 mg/mL,0.03~1 mg/mL和0.01~0.5 mg/mL时线性关系良好,平均加样回收率分别为96.8%,97.0%和96.4%,相对标准偏差(RSD)分别为1.53%,1.37%和1.96%。用该法同时检测了不同干旱条件处理下长春花样品中的文多灵、长春质碱和脱水长春碱,方法准确、快速、简便。  相似文献   

3.
As a prerequisite to the determination of pharmacokinetic parameters of icariin in rats, an HPLC method using UV detection was developed and validated. Icariin and the internal standard, quercetin, were extracted from plasma samples using ethyl acetate after acidification with 0.05 mol/L NaH2PO4 solution (pH 5.0). Chromatographic separation was achieved on an Agilent XDB Cls column (250 x 4.6 mm id, 5 microm) equipped with a Shim-pack GVP-ODS C18 guard column (10 x 4.6 mm id, 5 microm) using a mobile phase of ACN/water/acetic acid (31:69:0.4 v/v/v) at a flow rate of 1.0 mL/ min. Detection was at 277 nm. The calibration curve was linear from 0.05 to 100.0 microg/mL with 0.05 microg/mL as the lower LOQ (LLOQ) in plasma. The intra- and interday precisions in terms of RSD were lower than 5.7 and 7.8% in rat plasma, respectively. The accuracy in terms of relative error (RE) ranged from -1.6 to 3.2%. The extraction recoveries of icariin and quercetin were 87.6 and 80.1%, respectively. The main pharmacokinetic parameters for rats were determined after a single intravenous administration of 10 mg/kg icariin: t1/2, 0.562 +/- 0.200 h; AUC0-infinity, 8.73 +/- 2.23 microg x h/mL; CLToT, 20.10 +/- 5.80 L/kg x h; Vz, 1.037 +/- 0.631 L/kg; MRT0-infinity, 0.134 +/- 0.040 h; and Vss, 0.170 +/- 0.097 L/kg.  相似文献   

4.
Lawsone (1), lawsone methyl ether (2), and methylene-3,3'-bilawsone (3) are the main naphthoquinones in the leaf extracts of Impatiens balsamina L. (Balsaminaceae). Antimicrobial activities of these three naphthoquinones against dermatophyte fungi, yeast, aerobic bacteria and facultative anaerobic and anaerobic bacteria were evaluated by determination of minimal inhibitory concentrations (MICs) and minimal bactericidal or fungicidal concentrations (MBCs or MFCs) using a modified agar dilution method. Compound 2 showed the highest antimicrobial activity. It showed antifungal activity against dermatophyte fungi and Candida albicans with the MICs and MFCs in the ranges of 3.9-23.4 and 7.8-23.4?μg?mL(-1), respectively, and also had some antibacterial activity against aerobic, facultative anaerobic and anaerobic bacteria with MICs in the range of 23.4-93.8, 31.2-62.5 and 125?μg?mL(-1), respectively. Compound 1 showed only moderate antimicrobial activity against dermatophytes (MICs and MFCs in the ranges of 62.5-250 and 125-250?μg?mL(-1), respectively), but had low potency against aerobic bacteria, and was not active against C. albicans and facultative anaerobic bacteria. In contrast, 3 showed significant antimicrobial activity only against Staphylococus epidermidis and Bacillus subtilis (MIC and MBC of 46.9 and 93.8?μg?mL(-1), respectively).  相似文献   

5.
The composition of essential oil isolated from Satureja thymbra, growing wild in Libya, was analyzed by GC and GC-MS. The essential oil was characterized by γ-terpinene (39.23%), thymol (25.16%), p-cymene (7.17%) and carvacrol (4.18%) as the major constituents. Antioxidant activity was analyzed using the 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging method. It possessed strong antioxidant activity (IC50 = 0.0967 mg/mL). The essential oil was also screened for its antimicrobial activity against eight bacterial and eight fungal species, showing excellent antimicrobial activity against the microorganisms used, in particular against the fungi. The oil of S. thymbra showed bacteriostatic activity at 0.001-0.1 mg/mL and was bactericidal at 0.002-0.2 mg/mL; fungistatic effects at 0.001-0.025 mg/mL and fungicidal effects at 0.001-0.1 mg/mL. The main constituents thymol, carvacrol and γ-terpinene also showed strong antimicrobial activity. The commercial fungicide bifonazole showed much lower antifungal activity than the tested oil.  相似文献   

6.
The reversed-phase HPLC analysis of a methanol extract of the aerial parts of Cuscuta reflexa afforded a non-separable mixture (55 : 45) of two novel tetrahydrofuran derivatives, named swarnalin (1) and cis-swarnalin (2), and a known coumarin, 5,6,7-trimethoxycoumarin (3). The structures of the compounds were elucidated unequivocally by UV, HRFABMS and a series of 1D and 2D NMR analyses. The mixture of 1 and 2 showed significant free radical scavenging activity in the DPPH assay and the RC50 value was found to be 3.80 x 10(-4) mg mL(-1) for the mixture, compared to 2.88 x 10(-5) mg mL(-1) for the positive control, quercetin.  相似文献   

7.
Nanocontrast agents have great potential in magnetic resonance (MR) molecular imaging applications for clinical diagnosis. We synthesized Au(3)Cu(1) (gold and copper) nanoshells that showed a promising MR contrast effect. For in vitro MR images, the large proton r1 relaxivities brightened T(1)-weighted images. As for the proton-dephasing effect in T(2), Au(3)Cu(1) lightened MR images at the low concentration of 0.125 mg mL(-1) (3.84 x 10(-7) mM), and then the signal continuously decreased as the concentration increased. For in vivo MR imaging, Au(3)Cu(1) nanocontrast agents enhanced the contrast of blood vessels and suggested their potential use in MR angiography as blood-pool agents. We propose that (1) the cooperativity originating from the form of the nanoparticles and (2) the large surface area coordinated to water from their porous hollow morphology are important for efficient relaxivity. In a cytotoxicity and animal survival assay, Au(3)Cu(1) nanocontrast agents showed a dose-dependent toxic effect: the viability rate of experimental mice reached 83% at a dose of 20 mg kg(-1) and as much as 100% at 2 mg kg(-1).  相似文献   

8.
A new flow-injection procedure has been developed for the determination of salicylic acid based on the enhancement of the chemiluminescence from the cerium(IV)-Tween 20 reaction by salicylic acid in acidic medium. The method is simple, selective and sensitive with a detection limit of 2.5x10(-9) g mL(-1). It is applicable to the determination of salicylic acid in the concentration range of 4.0x10(-9)-1.1x10(-6) g mL(-1). The relative standard deviation (RSD) is 0.85% for 4.0x10(-7) g mL(-1) salicylic acid (n=11). The method has been successfully applied to the determination of salicylic acid in bactericidal solutions. Furthermore, it is suggested that light emission from cerium(IV)-Tween 20 reaction is probably because of the formation of singlet oxygen 1O2* and the emitter is excited oxygen molecular pairs O2(1delta(g))O2(1sigma(g)-).  相似文献   

9.
A sensitive and simple high-performance liquid chromatographic method with UV detection was developed and validated for the determination of andrographolide in rat whole blood. Carbamazepine was employed as internal standard and the blood sample was extracted with chloroform. Chromatographic separations were achieved on a Chromasil ODS column (250 x 4.6 mm, 5 microm). The mobile phase was consisted of methanol-water (52:48, v/v) and delivered at 0.8 mL/min. The detection wavelength was set at 225 nm. The calibration curve had a good linearity in the range 0.053-530 microg/mL in rat whole blood with its correlation coefficient being 0.996. The extraction recovery of andrographolide was ranged from 65.7 to 72.6%. The intra-day and inter-days repeatabilities were below 4.2% in terms of the percentage of relative standard deviation (RSD). The method was used to provide data on the pharmacokinetics of the drug in rats. The data obtained was processed using the 3P87 pharmacokinetic program. The results showed that the disposition of andrographolide after intravenous administration of liposomal andrographolide conformed to a two-compartment open model with alpha = 4.75 x 10(-2) +/- 2.41 x 10(-3) min(-1), beta = 3.16 x 10(-3) +/- 1.58 x 10(-4) min(-1), V(c) = 174.67 +/- 13.97 mL, k(21) = 1.60 x 10(-2) +/- 8.12 x 10(-4) min(-1), k(10) = 9.38 x 10(-3) +/- 5.62 x 10(-4) min(-1), k(12) = 2.53 x 10(-2) +/- 1.27 x 10(-3) min(-1) and AUC(0-infinity) = 1525.47 +/- 92.35 microg min/mL. For the intragastric administration of andrographolide tablets, the disposition of andrographolide followed a one-compartment open model with k(e) = 6.78 x 10(-3) +/- 3.53 x 10(-4) min(-1), k(a) = 3.69 x 10(-2) +/- 4.68 x 10(-3) min(-1), T(max) = 59.69 +/- 3.61 min, C(max) = 1.62 +/- 0.11 microg/mL, V(c) = 1056.90 +/- 83.42 mL, AUC(0-infinity) = 348.75 +/- 24.41 microg min/mL.  相似文献   

10.
A hyperbranched aliphatic polyester has been functionalized with PEG chains to afford a novel water-soluble BH40-PEG polymer which exhibits unimolecular micellar properties, and is therefore appropriate for application as a drug-delivery system. The solubility of the anticancer drug paclitaxel was enhanced by a factor of 35, 110, 230, and 355 in aqueous solutions of BH40-PEG of 10, 30, 60, and 90 mg x mL(-1), respectively. More than 50% of the drug is released at a steady rate and release is almost complete within 10 h. The toxicity of BH40-PEG was assessed in vitro with A549 human lung carcinoma cells and found to be nontoxic for 3 h incubation up to a 1.75 mg x mL(-1) concentration while LD50 was 3.5 mg x mL(-1). Finally, it was efficiently internalized in cells, primarily in the absence of foetal bovine serum, while confocal microscopy revealed the preferential localization of the compound in cell nuclei. [Figure: see text].  相似文献   

11.
Polymyxin-based combination therapy is commonly used to treat carbapenem-resistant Acinetobacter baumannii (CRAB) infections. In the present study, the bactericidal effect of polymyxin B and minocycline combination was tested in three CRAB strains containing blaOXA-23 by the checkerboard assay and in vitro dynamic pharmacokinetics/pharmacodynamics (PK/PD) model. The combination showed synergistic or partial synergistic effect (fractional inhibitory concentration index ≤0.56) on the tested strains in checkboard assays. The antibacterial activity was enhanced in the combination group compared with either monotherapy in in vitro PK/PD model. The combination regimen (simultaneous infusion of 0.75 mg/kg polymyxin B and 100 mg minocycline via 2 h infusion) reduced bacterial colony counts by 0.9–3.5 log10 colony forming units per milliliter (CFU/mL) compared with either drug alone at 24 h. In conclusion, 0.75 mg/kg polymyxin B combined with 100 mg minocycline via 2 h infusion could be a promising treatment option for CRAB bloodstream infections.  相似文献   

12.
The essential oil of Tibetan medicine Dracocephalum heterophyllum Benth was obtained by hydrodistillation with a 0.7% (v/w) yield. The chemical composition of the essential oil was analyzed by gas chromatography-mass spectral (GC-MS). Eighty-three compounds, constituting about 89.83% of the total oil, were identified. The main compound in the oil were Cineole (14.89%), trans-nerolido (7.10%), 1-m-ethyl-2-(1-methylethyl)-benzene (4.42%), Germacrene-D (4.84%), Decahydro-1,1,4,7-tetramethyl-4aH-cycloprop[e]azulen-4a-ol (4.94%), p-menth-1-en-4-ol,acetate (4.34%), 4-methyl-1-(1-methylethyl)-3-cyclohexen-1-ol (4.10%). The antimicrobial activity of the oil was evaluated against nine bacterial, one yeast, and three fungi. The antimicrobial test result showed that the essential oil strongly inhibited the growth of test microorganisms studied. The maximal inhibition zones and MIC values for bacterial, yeast and fungi strain were in the range of 18-25 mm and 0.039-0.156 mg mL(-1); *20 mm, and 0.156 mg mL(-1); 8-24 mm and 0.313-2.5 mg mL(-1); respectively. The antioxidant activity of the oil was determined by the malonyldialdehyde (MDA) test, measuring the MDA concentration in mouse liver cell microsomal after induced lipid peroxidation using FeSO(4) and ascorbic acid, The inhibition of lipid peroxidation was 59.3% with a concentration of 0.5 mg mL(-1). Result presented here may suggest that the essential oil of D. heterophyllum posses antimicrobial and antioxidant properties, and therefore, they can be one of new medicinal resources for antimicrobial agent and/or used as a natural preservative ingredient in food and cosmetics and pharmaceuticals industry.  相似文献   

13.
高效液相色谱法测定大鼠血浆中的原儿茶酸   总被引:3,自引:0,他引:3  
《色谱》2007,25(2):207-210
建立了大鼠血浆中原儿茶酸含量测定的高效液相色谱方法。采用的色谱柱为DiamondsilTM C18 柱(150 mm×4.6 mm,5 μm);流动相为乙腈-水(体积比为9∶91,用H3PO4 调pH至2.5);流速1.2 mL/min;检测波长260 nm;内标为对羟基苯甲酸。原儿茶酸的线性范围为0.050~3.20 mg/L,线性相关系数为0.9978,最低定量限为0.050 mg/L,日内和日间测定的精密度(以相对标准偏差表示)均低于7.0%,准确度(以相对误差表示)为-1.4%~2.6%;在0.050,0.40,3.20 mg/L低、中、高3个添加浓度水平下,血浆样品的提取回收率分别为83.4%,87.3%,91.1%。该方法简便,灵敏,准确,适用于大鼠体内原儿茶酸的药物动力学研究。  相似文献   

14.
Belaz KR  Cass QB  Oliveira RV 《Talanta》2008,76(1):146-153
The development and validation of a fully automated achiral-chiral high performance liquid chromatography (HPLC) method for the simultaneous determination of albendazole metabolites: enantiomers of albendazole sulphoxide (ABZ-SO), albendazole sulphone (ABZ-SO(2)) and albendazole 2-aminosulphone (ABZ-SO(2)NH(2)) in bovine plasma are described. This method involves an octyl restricted access media bovine serum albumin column (C(8)-RAM-BSA) (50 mm x 4.6 mm I.D.) for sample clean-up, followed by enantioselective analysis on a column containing an amylose tris(3,5-dimethylphenylcarbamate) stationary phase (150 mm x 4.6 mm I.D.). The chromatographic separations of all target compounds were performed at 30 degrees C using a mobile phase composed of phosphate buffer (10 mmol L(-1); pH 7.5):acetonitrile (60:40, v/v), flow rate of 0.5 mL min(-1) and fluorescence detection at 290 nm and 320 nm, excitation and emission, respectively. The influence of different organic modifiers and chiral selector of the stationary phase on enantioseparation of ABZ-SO was investigated. The method developed was fully validated. The calibration curves were linear in the concentration range of 40.00-1280 ng mL(-1) for each albendazole sulphoxide enantiomer, 10.0-320 ng mL(-1) for albendazole sulphone and 20.0-320 ng mL(-1) for albendazole 2-aminosulphone. The inter- and intra-day precision ranged from 0.760% to 7.79% relative standard deviation (R.S.D.), and the accuracy ranged 101% from 114% of the nominal values while the transfer efficiency was in the range of 84.4-103%. The method showed good linearity, precision, accuracy, sensitivity and selectivity allowing it to be appropriate for further pharmacokinetics and metabolism studies of albendazole.  相似文献   

15.
Kumar SA  Tang CF  Chen SM 《Talanta》2008,76(5):997-1005
We report a new method for selective determination of acetaminophen (AP) in physiological condition. A new hybrid film modified electrode was fabricated using inorganic semiconducting nano-TiO(2) particles and redox active polymer. Redox polymer, poly(acid yellow 9) (PAY) was electrochemically deposited onto nano-TiO(2) coated glassy carbon (GC) electrode. Surface characterizations of modified electrode were investigated by using atomic force microscope and scanning electron microscope. The PAY/nano-TiO(2)/GC hybrid electrode shows stable redox response in the pH range 1-12 and exhibited excellent electrocatalytic activities towards AP in 0.1M phosphate buffer solution (pH 7.0). Consequently, a simple and sensitive electroanalytical method was developed for the determination of AP. The oxidation peak current was proportional to the concentration of acetaminophen from 1.2 x 10(-5) to 1.20 x 10(-4)M and the detection limit was found to be 2.0 x 10(-6)M (S/N=3). Possible interferences were tested and evaluated that it could be possible to selective detection of AP in the presences of dopamine, nicotinamide adenine dinucleotide (NADH), ascorbic acid and uric acid. The proposed method was used to detect acetaminophen in commercial drugs and the obtained results are satisfactory.  相似文献   

16.
Zhou L  Li D  Wang J  Liu Y  Wu J 《Natural product research》2007,21(4):283-291
This study was to isolate antibacterial compounds from Gleditsia sinensis Lam. spines through bioassay-guided fractionation (against a Gram-positive bacterium Xanthomonas vesicatoria and a Gram-negative bacterium Bacillus subtilis). The crude ethanol extract of G. sinensis spines was partitioned sequentially with solvents of increasing polarity. The ethyl acetate fraction, which exhibited the most significant antibacterial activities among all the solvent fractions, was further separated by column chromatograph, yielding seven phenolic compounds including ethyl gallate (1) and caffeic acid (7), and five flavonoids, dihydrokaempferol (2), eriodictyol (3), quercetin (4), 3,3',5',5,7-pentahydroflavanone (5) and (-)-epicatechin (6). Compounds 4, 5 and 7 showed moderate inhibitory activities against both bacterial species, with compound 7 having the lowest minimal inhibitory concentration (MIC) of 0.125 mg mL(-1), while compounds 1 and 2 showed a weak inhibitory activity only against B. subtilis (MIC 1.00 mg mL(-1)), and compounds 3 and 6 showed insignificant activity against the two bacteria.  相似文献   

17.
A rapid and specific HPLC method was developed and validated for simultaneous determination of diazepam and its main active metabolites, desmethyldiazepam, oxazepam and temazepam in human plasma. Plasma samples were extracted using toluene. HPLC system included a Chromolith Performance RP-18e 100 mm x 4.6mm column, using 10mM phosphate buffer (pH 2.5)-methanol-acetonitrile (63:10:27, v/v) as mobile phase running at 2 mL min(-1). UV detector (lambda=230 nm) was used. The calibration curves were linear in the concentration range of 2-800 ng mL(-1) for diazepam and 2-200 ng mL(-1) for the three metabolites (r(2)>0.99). The lower limit of quantification was 2 ng mL(-1) for all analytes. Within and between-day precisions in the measurement of QC samples were in the range of 1.8-18.0% for all analytes. The developed procedure was used to assess the pharmacokinetics of diazepam and its main metabolites following single dose administration of 10mg diazepam orally to healthy subjects.  相似文献   

18.
Active catalysts for water oxidation to evolve O(2) are required for the construction of artificial photosynthetic devices that are expected to be promising energy-providing systems in the future. The citrate-stabilized IrO(2) colloid was self-assembled onto an indium tin oxide (ITO) electrode to form a monolayer of the colloidal IrO(2) particles when it was dipped in the colloid solution. The self-assembly could be achieved by a chemical interaction between carboxylate groups on the citrate stabilizer and hydroxyl groups on the ITO surface to form ester bonds. Efficient electrocatalysis for water oxidation was demonstrated using the electrode modified by the self-assembled IrO(2) colloid to yield the highest turnover frequency ((2.3-2.5) x 10(4) h(-1)) of IrO(2) in the hitherto-reported catalysts for electrochemical water oxidation.  相似文献   

19.
设计并制作了一种集多孔流分离(Multi-orifice flow fractionation,MOFF)技术与磁捕获技术于一体的用于特异性分离和捕获合成样本中肝癌细胞HepG2的多功能微流控细胞芯片.此芯片由玻璃基片和PDMS微通道盖片组成,PDMS盖片上含有3条进样通道、MOFF分离区和六边形腔体的细胞富集检测区.其中,MOFF分离区总长20 mm,由80组长度为0.18 mm、深度为50μm、收缩区域宽度为0.06 mm、扩张区域宽度为0.20 mm的半菱形收缩/扩张重复单元组成,每组收缩/扩张重复单元间的夹角为103.0°.实验以肝癌细胞HepG2-血细胞混悬液为样本;根据磁珠表面修饰c-Met抗体能与肝癌细胞HepG2特异性结合的原理,通过表面羧基化的磁珠、EDC(1 mg/mL)、NHS(1 mg/mL)和c-Met抗体制备了浓度为50μg/mL的免疫磁珠(Anti-MNCs)悬浮液.在样本流速为50μL/min条件下,利用外加磁场实现了血细胞合成样本中微量肝癌细胞HepG2的有效捕获;采用微波加热法以柠檬酸、硫脲为原料制备了用于荧光标记HepG2的碳量子点,在芯片上实现了血液中肝癌细胞HepG2的原位荧光可视化观测.对芯片检测区捕获到的HepG2进行了显微计数分析,对500μL血细胞(107 cell/mL)中含10个HepG2细胞的合成样本,捕获效率达到88.5%±6.7%(n=20).结果表明,所设计的多模式多功能的微流控芯片具有良好的肿瘤细胞分离和检测功能.  相似文献   

20.
A new cytotoxic himachalene sesquiterpenoid 4alpha-methoxy-5,9-oxahimachal-9-ene (hugonianene A) which exhibited moderate activity against Anopheles gambiae mosquito larvae after 24 h at a concentration of 0.237 mg mL(-1), and at 48 h and 72 h contact time causing complete larval mortality up to a concentration as low as 0.01369 mg mL(-1), was isolated as the major constituent of the cytotoxic root bark extract of Hugonia busseana. Hugonianene A was obtained together with the hitherto unreported rosane diterpenoid 18-hydroxyrosane, the known rosane diterpenoid hugorosediol, an inseparable mixture of 12-methoxy-13-methylpodocarpa-8,11,13-trien-3,7-dione and 12-methoxy-13-methylpodocarpa-1,8,11,13-tetraen-3,7-dione, and the di-podocarpanoid hugonone B that was previously obtained from H. castaneifolia.  相似文献   

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