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以2,7-二溴-9,9-二苯基芴为起始原料,采用发散合成策略,合成了一种新型三苯胺树枝状分子--2,7-二[N,N-二(4-二苯胺基苯基)胺基]-9,9-二苯基芴(FTPA),其结构经1H NMR, 13C NMR, HR-MS和元素分析表征。并对热稳定性、光谱性质和电化学性质进行了研究。结果表明:FTPA的热分解温度和玻璃化转变温度分别为592 ℃和154 ℃; FTPA的吸收峰位于309 nm, 349 nm和409 nm,最大发射波长为465 nm; FTPA的第一、第二及第三氧化电势分别为0.37 V, 0.49 V和0.83 V。 相似文献
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通过双Suzuki偶联反应一步合成了2种含硫甲基的芴-苯结构化合物2,7-二(4-硫甲基苯基)-9,9-二己基-芴(a)和2,7-二(2,6-二甲基-4-硫甲基苯基)-9,9-二己基-芴(b).紫外-可见和荧光光谱以及分子轨道理论计算表明,位阻较小的化合物a具有更好的共轭性能,其最大紫外-可见吸收波长达到351nm,比两端苯基含4个邻位取代基的化合物b红移了38nm;化合物a的最大荧光发射波长达到410nm,为典型的蓝光化合物,比化合物b红移了43nm.化合物a和b都具有较高的荧光量子产率,分别为59%和65%,在光电材料方面具有潜在的应用前景. 相似文献
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A simple, rapid, and sensitive HPLC method based on 9H‐fluoren‐9‐ylmethyl chloroformate derivatization for the quantification of sertraline in rat plasma has been developed, requiring a plasma sample of only 0.1 mL, which was deproteinized and derivatized for 5 min in two single steps. The obtained derivative was stable at room temperature and was determined by HPLC using a fluorescence detector. The analytical column was a C(18) column and the mobile phase was acetonitrile and water (80:20, v/v). Calibration curves were linear in the range of 10–500 ng/mL. The limit of detection was approximately 3 ng/mL, and the lower limit of quantification was established at 10 ng/mL. The bias of the method was lower than 10%, and the within day as well as between day, relative standard deviations were lower than 12%. This analytical method was successfully applied to characterize sertraline pharmacokinetics in rats following intravenous (t1/2 = 213 ± 48 min, Cl = 43.1 ± 8.7 mL/min, Vd = 11560 ± 1861 mL) and oral (Cmax = 156 ± 76 ng/mL, tmax = 63.8 ± 16.3 min) administration of 2 and 5 mg, respectively. 相似文献
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Detection of α‐Methylacyl‐CoA Racemase in Serum and Urine Using a Highly Sensitive Electrochemical Immunodetector 下载免费PDF全文
The detection of α‐methylacyl‐CoA racemase (AMACR), a novel biomarker for prostate cancer, is demonstrated in serum and urine using a novel immuno‐detection method. The detection system consists of a three‐electrode conventional electrochemical cell modified with a gating electrode for applying a gating voltage VG to the immune complex immobilized on the working electrode to provide signal amplification. The detection system is realized by integrating gating electrodes with screen‐printed electrodes. This detection method does not require involved sample preparation procedures. The detection was demonstrated in serum and urine samples on the nanogram/mL level with VG equal to 0.6 V. Detection in serum was also performed on the picogram/mL level with a limit of 100 picogram/mL with VG=0.6 V being a necessary condition. 相似文献
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Sevgi Tatar Ulu 《中国化学》2012,30(3):634-638
A simple, rapid and sensitive high performance liquid chromatography (HPLC) method was developed for the determination of metoclopramide in pharmaceutical preparation. The method is based on the derivatization of metoclopramide with fluorescamine. The separation was achieved on a C18 column using methanol‐water (70:30, V/V) mobile phase. Fluorescence detector was used at the excitation and emission of 403 and 485 nm, respectively. The method was validated for linearity, limit of detection, limit of quantification, precision, accuracy, recovery, robustness and system suitability. The assay was linear over the concentration range of 100–2000 ng/mL. The mean recovery was 100.37%. The proposed method was successfully applied to the assay of metoclopramide in tablet preparation. The preparation was also analyzed with an official method and statistical comparison by t‐ and F‐tests revealed that there was no significant difference between the results of the two methods with respect to mean values and standard deviations at the 95% confidence level. 相似文献
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Casey L. Sayre Yangmiao Zhang Stephanie E. Martinez Jody K. Takemoto Neal M. Davies 《Biomedical chromatography : BMC》2013,27(5):548-550
The complete pharmacokinetic disposition of the chiral flavonoid (±) pinostrobin remains unknown without the development of an analytical method of detection and quantitation of its individual enantiomers. Resolution of the enantiomers of pinostrobin was achieved using as simple high‐performance liquid chromatographic method. A Chiralpak® AD‐RH column was employed to perform baseline separation with UV detection at 287 nm. The standard curves were linear ranging from 0.5 to 100 µg/mL for each enantiomer. The limit of quantification was 0.5 µg/mL. Precision and accuracy of the assay was < 15% (RSD) and was with a bias <15% for all points on the calibration curve. The assay was applied successfully to stereoselective serum disposition of pinostrobin enantiomers in rats. Both enantiomers had a serum half‐life of ~7 h. They also shared similar values of volume of distribution (Vd S‐pinostrobin, 8.2 L/kg; Vd R‐pinostrobin, 8.9 L/kg), total clearance (S‐pinostrobin CLtotal, 0.959 L//h/kg; R‐pinostrobin CLtotal, 1.055 L//h/kg), and area under the curve (S‐pinostrobin AUCinf, 23.16 µg h/mL; R‐pinostrobin AUCinf, 21.296 µg h/mL). The large volume of distribution suggests extensive distribution of pinostrobin into tissues. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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Johnique Billups Cynthia Jones Tanise L. Jackson Seth Y. Ablordeppey Shawn D. Spencer 《Biomedical chromatography : BMC》2010,24(7):699-705
A simple and rapid RP‐HPLC‐DAD method was developed and validated for simultaneous determination of the dopamine antagonists haloperidol, its diazepane analog, and the dopamine agonist bromocriptine in rat plasma, to perform pharmacokinetic drug‐interaction studies. Samples were prepared for analysis by acetonitrile (22.0 μg/mL) plasma protein precipitation with droperidol as an internal standard, followed by a double‐step liquid‐liquid extraction with hexane : chloroform (70:30) prior to C‐18 separation. Isocratic elution was achieved using a 0.1% (v/v) trifluoroacetic acid in deionized water, methanol and acetonitrile (45/27.5/27.5, v/v/v). Triple‐wavelength diode‐array detection at the λmax of 245 nm for haloperidol, 254 nm for the diazepane analog and droperidol, and 240 nm for bromocriptine was carried out. The LLOQ of DAL, HAL, and BCT were 45.0, 56.1, and 150 ng/mL, respectively. In rats, the estimated pharmacokinetic parameters (i.e., t1/2, CL, and Vss) of HAL when administered with DAL and BCT were t1/2 = 16.4 min, Vss = 0.541 L/kg for HAL, t1/2 = 28.0 min, Vss = 2.00 L/kg for DAL, and t1/2 = 24.0 min, Vss = 0.106 L/kg for BCT. The PK parameters for HAL differed significantly from those previously reported, which may be an indication of a drug‐drug interaction. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
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A method for analysis of short-chain chlorinated paraffins (SCCPs) in water based on solid-phase extraction (SPE) was established using electron capture negative chemical ionization mass spectrometry (GC-ENCI-MS). The SPE parameters, including the sorbent, eluent and elution volume were optimized. The Agilent Bond Elut-C18 was precleaned with 3 mL of hexane and 3 mL of methanol, and subsequently conditioned with 3 mL H2O prior to use. After the water samples were enriched by the cartridge, the sample was washed with 3 mL of 10% (V/V) methanol and eluted with 3 mL of hexane-dichloromethane (1:1, V/V) solution. The results indicated that the limits of detection (LOD) for SCCPs were 18 ng L?1, while the corresponding limits of quantitation (LOQ) were 60 ng L?1. The spiked recovery range was 90%–135%, with a relative standard deviation of less than 10%. Finally, 20 surficial water samples around Beijing were collected and SCCPs contents were analyzed using the proposed method. The SCCPs concentrations ranged from less than LOD to 682 ng L?1 with a mean concentration of 216 ng L?1. 相似文献
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A new analytical method for phenylpropanolamine based on micellar electrokinetic chromatographic separation and laser‐induced fluorescence detection has been developed. Naphthalene‐2,3‐dicarboxaldehyde was used for precolumn derivatization of the nonfluorescent drug. Optimal separation and detection were obtained with an electrophoretic buffer of 50 mM sodium borate (pH 9.5) containing 15 mM sodium dodecyl sulfate and a He‐Cd laser (Δex: 442 nm, Δem: 500 nm). Linearity (r ≥ 0.99) of two orders of magnitude was generally obtained and the concentration limit of detection was in the ng/mL level. Coupled with a simple cleanup procedure, the method can be applied to the analysis of phenylpropanolamine in human plasma, with a limit of detection at 15 ng/mL. Recovery of phenylpropanolamine from plasma samples was about 90%. 相似文献
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《Analytical letters》2012,45(1):18-28
A simple and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous analysis of three tropane alkaloids in blood and urine. After 1 mL of a blood or urine sample was extracted using a liquid–liquid extraction method with ethyl acetate at pH 8 and homatropine as the internal standard, the tropane alkaloids were separated. An Allure PFP propyl column (50 mm × 2.1 mm, 5 µm) separated the tropane alkaloids using an acetonitrile-buffer solution (20 mmol/L ammonium acetate and 0.1% formic acid, pH 4) (70:30) as the mobile phase at a flow-rate of 0.2 mL/min in isocratic mode, with the LC-MS/MS in the positive ionization mode. For each compound, detection was related to two daughter ions (scopolamine: m/z 304.4 → 138.1 and 155.9; atropine: m/z 290.3 → 124.0 and 93.1; anisodamine: m/z 306.3 → 140.1 and 91.1; and homatropine: m/z 276.3 → 124.3 and 142.1). The tropane alkaloids exhibited excellent linearity in the range of 0.05–100 ng/mL in blood and 0.2–100 ng/mL in urine, with a limit of detection range from 0.02 to 0.05 ng/mL for biological materials. The extraction recoveries of atropine, scopolamine, and anisodamine were more than 53% in the blood and urine; the interday and intraday RSDs were less than 10%; the within-day and between-day accuracy were between ?9.8% and +8.8%. The present method is simple and rapid, as shown by its application to a clinical case. This method is useful for routine analysis of tropane alkaloids in cases of suspected tropane alkaloid poisoning. 相似文献
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Ranjeet Kaur Satyanshu Kumar Arnab Chatterjee Sunil K Chattopadhyay 《Biomedical chromatography : BMC》2010,24(9):1000-1005
A simple, rapid, accurate and reproducible reverse‐phase HPLC method has been developed for simultaneous identification and quantification of three coumarinolignoids, cleomiscosin A (Cliv A), cleomiscosin B (Cliv B) and cleomiscosin C (Cliv C) in different extracts of the seeds of Cleome viscosa using photodiode array detection at 326 nm. Cliv A, B and C were separated on a Waters symmetry C18 column (250 × 4.6 mm, 5 μm) using the solvent system consisting of a mixture of acetonitrile : methanol (1:2 v/v) and water : acetic acid (99.5:0.5 v/v) as a mobile phase in a gradient elution mode. The calibration curves were linear in the concentration ranges 15–200, 10–80 and 15–180 μg/mL for Cliv A, Cliv B and Cliv C, respectively. The limits of detection and quantification for Cliv A, Cliv B and Cliv C were 15 and 20 μg/mL, 10 and 15 μg/mL and 15 and 20 μg/mL, respectively. The intra‐day and inter‐day precisions were 2.08 and 0.93% for Cliv A , 1.22 and 0.39% for Cliv B and 1.29 and 0.23 for Cliv C respectively. The developed HPLC method was used to identify and quantify Cliv A, Cliv B and Cliv C in different extracts of seed of Cleome viscosa. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
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Arnab Chatterjee Satyanshu Kumar Sunil K. Chattopadhyay 《Biomedical chromatography : BMC》2013,27(12):1720-1725
A simple, rapid, accurate and reproducible reverse‐phase HPLC method has been developed for the identification and quantification of two alkaloids ephedrine and cryptolepine in different extracts of Sida species using photodiode array detection. Baseline separation of the two alkaloids was achieved on a Waters RP‐18 X‐terra column (250 × 4.6 mm, 5 µm) using a solvent system consisting of a mixture of water containing 0.1% Trifluoroacetic acid (TFA) and acetonitrile in a gradient elution mode with detection at 210 and 280 nm for ephedrine and cryptolepine, respectively. The calibration curves were linear in a concentration range of 10–250 µg/mL for both the alkaloids with correlation coefficient values >0.99. The limits of detection and quantification for ephedrine and cryptolepine were 5 and 10 µg/mL and 2.5 and 5 µg/mL, respectively. Relative standard deviation values for intra‐day and inter‐day precision were 1.22 and 1.04% for ephedrine and 1.71 and 2.06% for cryptolepine, respectively. Analytical recovery ranged from 92.46 to 103.95%. The developed HPLC method was applied to identify and quantify ephedrine and cryptolepine in different extracts of Sida species. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献