全文获取类型
收费全文 | 1443篇 |
免费 | 169篇 |
国内免费 | 86篇 |
专业分类
化学 | 1632篇 |
晶体学 | 7篇 |
力学 | 3篇 |
综合类 | 6篇 |
数学 | 8篇 |
物理学 | 42篇 |
出版年
2024年 | 6篇 |
2023年 | 18篇 |
2022年 | 92篇 |
2021年 | 42篇 |
2020年 | 94篇 |
2019年 | 106篇 |
2018年 | 83篇 |
2017年 | 89篇 |
2016年 | 78篇 |
2015年 | 104篇 |
2014年 | 76篇 |
2013年 | 147篇 |
2012年 | 110篇 |
2011年 | 92篇 |
2010年 | 77篇 |
2009年 | 73篇 |
2008年 | 90篇 |
2007年 | 78篇 |
2006年 | 47篇 |
2005年 | 43篇 |
2004年 | 29篇 |
2003年 | 33篇 |
2002年 | 19篇 |
2001年 | 11篇 |
2000年 | 9篇 |
1999年 | 7篇 |
1998年 | 4篇 |
1997年 | 6篇 |
1996年 | 11篇 |
1995年 | 6篇 |
1994年 | 5篇 |
1993年 | 3篇 |
1992年 | 1篇 |
1990年 | 2篇 |
1989年 | 2篇 |
1988年 | 1篇 |
1986年 | 3篇 |
1985年 | 1篇 |
排序方式: 共有1698条查询结果,搜索用时 75 毫秒
101.
Ju Wang Wei Yao Di Fan Zhenjun Qiu Jieqiong Song Kai Pan Taijun Hang 《Biomedical chromatography : BMC》2019,33(10)
HR011303 is a novel and highly selective urate transporter 1 (URAT1) inhibitor. In this study, a sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for quantification of HR011303 in beagle dog plasma. Plasma samples were pretreated with protein‐precipitation extraction by acetonitrile and added with a trifluoromethyl substituted analog of HR011303 as internal standard. The chromatographic separation was performed on a Shiseido C18 column (100 × 4.6 mm, i.d., 5 μm) by mobile phases consisting of 5 mm ammonium–formic acid (100:0.1) and acetonitrile–formic acid (100:0.1) solutions in gradient elution. The MS detection was conducted in electrospray positive ionization with multiple reactions monitoring at m/z 338 → 240 for HR011303 and m/z 328 → 230 for the internal standard using 25 eV argon gas collision induced dissociation. The established LC–MS/MS method showed good selectivity, sensitivity, precision and accuracy. The plasma pharmacokinetics of HR011303 in beagle dogs following both oral and intravenous administration were then successfully evaluated using this LC–MS/MS method. 相似文献
102.
Résumé The solubility and rate of dissolution of a poorly-soluble active principle are of importance when substances are destined
for oral administration. Physical blends in wich drug and carrier are able to form particular compositions, such as a eutectic,
may exibit an increased rate of dissolution. In this work the interactions lorazepam and PEG 6000, were examined, the particular
thermal behaviour of lorazepam being taken into account. An eutectic was obtained and its composition was studied by means
of differential scanning calorimetry, thermomicroscopy, infrared spectroscopy and X-ray methods.
Zusammenfassung Bei der oralen Darreichung von Substanzen ist die L?slichkeit und Aufl?sungsgeschwindigkeit schlechtl?slicher aktiver Komponenten von gro?er Bedeutung. Physikalische Gemische, in denen Wirkstoffe und Tr?gersubstanzen besondere Zusammensetzungen wie zum Beispiel Eutektika zu bilden in der Lage sind, k?nnen eine erh?hte Aufl?sungsgeschwindigkeit zeigen. Vorliegend wird die Wechselwirkung zwischen Lorazepam und PEG 6000 untersucht, wobei das besondere thermische Verhalten von Lorazepam berücksichtigt wurde. Es wurde ein Eutektikum erhalten und dessen Zusammensetzung mittels DSC, Thermomikroskopie, Infrarotspektroskopie und R?ntgenmethoden untersucht.相似文献
103.
Casey L. Sayre Mandi Hopkins Jody K. Takemoto Neal M. Davies 《Biomedical chromatography : BMC》2013,27(3):404-406
Pharmacometric characterization studies of liquiritigenin have historically overlooked its chiral nature. To achieve complete characterization, an analytical method enabling the detection and quantification of the individual enantiomers of racemic (±) liquiritigenin is necessary. Resolution of the enantiomers of liquiritigenin was achieved using a simple high‐performance liquid chromatographic method. A Chiralpak® ADRH column was employed to perform baseline separation with UV detection at 210 nm.The standard curves were linear ranging from 0.5 to 100 µg/mL for each enantiomer. Limit of quantification was 0.5 µg/mL. The assay was applied successfully to stereoselective serum disposition of liquiritigenin enantiomers in rats. Liquiritigenin enantiomers were detected in serum as both aglycones and glucuronidated conjugates. Both unconjugated enantiomers had a serum half‐life of ~15 min in rats. The volume of distribution (Vd) for S‐ and R‐liquiritigenin was 1.49 and 2.21 L/kg, respectively. Total clearance (Cltotal) was 5.12 L/h/kg for S‐liquiritigenin and 4.79 L/h/kg for R‐liquiritigenin, and area under the curve (AUC0‐inf) was 3.95 µg h/mL for S‐liquiritigenin and 4.23 µg h/mL for R‐liquiritigenin. The large volume of distribution coupled with the short serum half‐life suggests extensive distribution of liquiritigenin into tissues. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
104.
Chiral analytical method development and application to pre‐clinical pharmacokinetics of pinocembrin
Casey L. Sayre Jody K. Takemoto Stephanie E. Martinez Neal M. Davies 《Biomedical chromatography : BMC》2013,27(6):681-684
An analytical method enabling the detection and quantification of the individual enantiomers of racemic (±) pinocembrin is required to fully characterize its pharmacokinetic disposition. Direct resolution of the enantiomers of pinocembrin was achieved using a novel and simple reversed‐phase high‐performance liquid chromatography method with electrospray ionization and detection by mass spectrometry in rat serum. A Chiralcel® AD‐RH column was employed to perform baseline separation with electrospray positive‐mode ionization with selected ion monitoring detection. The standard curves were linear from 0.5 to 100 µg/mL for each enantiomer. The limit of quantification was 0.5 µg/mL. The assay was applied successfully to stereoselective serum disposition of pinocembrin enantiomers in rats. Pinocembrin enantiomers were detected in serum. Both enantiomers had a serum half‐life of ~15 min in rats. Similar values of volume of distribution between the enantiomers were also observed: 1.76 L/kg for S‐pinocembrin and 1.79 L/kg for R‐pinocembrin. Total clearance was 5.527 L//h/kg for S‐pinocembrin and 5.535 L/h/kg for R‐pinocembrin, and the area under the curve was 1.821 µg h/mL for S‐pinocembrin and 1.876 µg h/mL for R‐pinocembrin. The large volume of distribution coupled with the short serum half‐life suggests extensive distribution of pinocembrin into the tissues. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
105.
A selective and sensitive liquid chromatography tandem mass spectrometry method (LC‐MS/MS) was developed and validated for the determination of cefdinir in rat plasma and urine. Following a simple protein precipitation using methanol, chromatographic separation was achieved with a run time of 10 min using a Synergi 4 µ polar‐RP 80A column (150 × 2.0 mm, 4 µm) with a mobile phase consisting of 0.1% formic acid in water and methanol (65:35, v/v) at a flow rate of 0.2 mL/min. The protonated precursor and product ion transitions for cefdinir (m/z 396.1 → 227.2) and cefadroxil, an internal standard (m/z 364.2 → 208.0) were monitored in the multiple reaction monitoring in positive ion mode. The calibration curves for plasma and urine were linear over the concentration range 10–10,000 ng/mL. The lower limit of quantification was 10 ng/mL. All accuracy values were between 95.1 and 113.0% and the intra‐ and inter‐day precisions were <13.0% relative standard deviation. The stability under various conditions in rat plasma and urine was also found to be acceptable at three concentrations. The developed method was applied successfully to the pharmacokinetic study of cefdinir after oral and intravenous administration. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
106.
不锈钢金属丝网上TiO2纳米薄膜光催化剂的研究 总被引:21,自引:0,他引:21
以钛酸正丁酯为原料,采用溶胶-凝胶法在金属丝网上制备了TiO2薄膜光催化剂.利用SEM,TEM,AES和Raman光谱研究了薄膜的表面及结构特性.以甲醛的光催化氧化反应为试验反应,考察了提拉次数、PEG浓度和焙烧温度对TiO2薄膜光催化剂活性的影响.将TiO2薄膜的结构特性与其光催化活性进行了关联.结果表明,在前驱体溶胶中加入10%PEG400,提拉3次并于400℃下焙烧可制得具有中孔结构和结晶完好的锐钛矿型TiO2薄膜,并具有最佳的光催化活性. 相似文献
107.
108.
A fast and sensitive high performance liquid chromatography method for quantitative determination of rosiglitazone in human plasma has been developed. The extraction from plasma was performed using solid-phase extraction (SPE) on C4 silica (100 mg) disposable extraction cartridges (DEC). The separation of rosiglitazone and two metabolites was achieved on a Phenomenex® Synergi 4 µm MAX-RP (150 × 4.6 mm) column, protected by a guard column. The mobile phase was 0.01 M ammonium acetate, pH 7.0 - acetonitrile (65:35, v/v). (3S)-3-OH-quinidine was used as internal standard. The analytes were detected using fluorescence detection. The method was validated. The limit of quantitation was 1 ng mL−1 and the detection limit was 0.25 ng mL−1 for rosiglitazone in human plasma. The recovery was 90% for rosiglitazone. Linearity was observed over a range of 1-1000 ng mL−1 (r2=0.9959). The intra- and inter-day precision (C.V.) did not exceed 8.7 %. Applicability of the method was demonstrated by a clinical pharmacokinetic study. A healthy volunteer received in two separate phases 4 mg and 8 mg rosiglitazone maleate as a single oral dose. Plasma concentrations were measured for 24 h in both phases. 相似文献
109.
Grafting polymer glycols onto nano-silica surface through one-step procedure was investigated. The major characteristic of this procedure is that all the materials and reagents (silica, PEG, TDI, DBTDL, solvent) required for grafting were added simultaneously into the reaction vessel. TDI and DBTDL were used as coupling agent and catalyst, respectively.The products were characterized by FTIR, TGA, elemental analyses and TEM, giving evidence for successful grafting of PEG. Possible mechanism of this grafting was studied and two grafting processes were proposed. The process through which the grafting proceeds depends on the reaction temperature. Effect of molecular weight of PEG on grafting was also investigated. 相似文献
110.
A soluble polymer-supported synthesis of indoles via palladium-mediated heteroannulation of terminal alkynes with o-iodoanilines has been described. The protocol provides a useful tool for constructing combinatorial indole libraries. 相似文献