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91.
目的 建立超高效液相色谱-串联质谱同时测定黄芩清热除痹胶囊中6种成分(黄芩苷、栀子苷、木犀草素、齐墩果酸、薏苡素、苦杏仁苷)含量的方法。方法 采用Phenomenex Luna Omega C18色谱柱(100 mm×2.1 mm,1.6 μm),以含10 mmol/L甲酸铵的0.1%甲酸水溶液(A)-0.1%甲酸的乙腈(B)为流动相,进行梯度洗脱,柱温为30 ℃,流速为0.25 mL/min,进样量5 μL,分析时间10 min。采用电喷雾离子源,以多反应监测模式在负离子条件下进行检测。结果 所测6种活性成分在测定浓度范围内线性关系良好(r≥0.999 0),精密度、稳定性和重复性良好,平均加样回收率为98.62%~103.7%,RSD≤2.70%。结论 该方法准确度高、分析速度快、检测限低、重复性高,适用于黄芩清热除痹胶囊质量控制。 相似文献
92.
A critical point of comparison between a fiber collected from a crime scene and a fiber from a known source is the color. Fiber dye analysis using thin-layer chromatography or ultraviolet (UV)-visible (Vis) microspectrophotometry provides useful, although limited, data for comparison. High-performance liquid chromatography-electrospray ionization mass spectrometry (LC/MS) overcomes these limitations by integrating chromatography, ultraviolet-visible spectroscopy, and mass spectrometry into a single instrument. In order to evaluate the applicability of the LC/MS to forensic fiber dye analysis, a multi-stage chromatographic method using acidified water and acidified acetonitrile was developed that separated and identified a mixture of 15 basic and 13 disperse dye standards. The LC/MS also detected and analyzed dyes extracted from individual 0.5 cm acrylic and polyester fibers, demonstrating its applicability to this type of analysis. With regard to the analysis of disperse dyes in polyester fibers, the replacement of pyridine with acetonitrile in the extraction system allowed direct injection of the extracts into the LC/MS. The advantage of the LC/MS over other instrumental methods of textile dye analysis is demonstrated by the analysis and differentiation of three black acrylic fibers: two fibers had similar UV-Vis spectra but were differentiated with chromatography and two had similar UV-Vis spectra and chromatograms but were differentiated using the mass spectrometer. 相似文献
93.
94.
目的建立肝中杀鼠酮的硅藻土提取方法和高效液相色谱检测法。方法取0.5g肝匀浆,加69/5HC10。沉淀蛋白,准确取1/2上清液倒入装有3.1g硅藻土的层析柱中,用10mL二氯甲烷或乙醚洗脱,洗脱液中加入安定作为内标,水浴浓缩,用0.2mL甲醇定容,供高效液相色谱分析。结果提取率分别为98.1%和99.9%,检出限分别为14ng/mL和13ng/mL。结论该方法简便、快速、提取率高,可作为法医毒物常规检测手段。 相似文献
95.
96.
Mercer JW Oldfield LS Hoffman KN Shakleya DM Bell SC 《Journal of forensic sciences》2007,52(2):383-388
This paper describes two analytical techniques used to separate and quantify gamma-hydroxybutyrate (GHB) and gamma-hydroxyvalerate (GHV). The first technique was a N,O-bis(trimethylsilyl)triflouro-acetimide-trimethylchlorosilane derivatization, followed by gas chromatography/mass spectrometry analysis using an HP-5 capillary column at a rate of 1.0 mL/min with a run time of 9.25 min. This technique was found to be sensitive (LOD 1 pg on column) and gave a low average error (5%) in a beverage study. When supplemented by a surrogate spike, the method yielded 97% analyte recovery from beverages. The second technique was high-performance liquid chromatography/UV (HPLC/UV) using a C-18 column with a (20:80% v/v) methanol:dibasic phosphoric buffer (10 mM, pH 3) at a rate of 1.00 mL/min with a run time of 7.5 min. UV detection occurred at 254 nm. This method was found to be less sensitive (LOD 0.05 microg on column) for direct analysis of aqueous samples. To remove interferences seen in the beverage study, a liquid-liquid extraction before HPLC analysis was tested. However, a decreased sensitivity (LOD 100 microg on column) and irreproducible peak profiles resulted. 相似文献
97.
目的:建立肠炎宁口服液中没食子酸含量测定方法.方法:采用高效液相色谱法(HPLC),色谱柱:Hypersil ODS C18(4.6 mm×150 mm);检测波长:271 nm;流动相:甲醇 0.5 g/L磷酸(5∶95);流速:1.0 ml/min.结果:没食子酸浓度为43.920~307.442 μg/ml时,与峰面积线性关系良好,平均回收率为100.2%,RSD为1.52%.结论:HPLC法准确、简便、快速,适合于该制剂的质量控制. 相似文献
98.
Abstract: Illicit distribution of various illicit or counterfeit drugs containing sildenafil and tadalafil has increased and caused noticeable problems in Korea. This study has been performed to determine the content range of sildenafil and tadalafil in various fake drugs. Among the illicit or counterfeit drugs seized by Korean authorities, 105 exhibits were used for the quantification. HPLC–UV analysis of methanol extractions was used for separation and quantitation of the two target compounds. The most abundant type of fake drug was counterfeit Viagra® tablets. Sildenafil was found in 73 exhibits, and tadalafil was found in seven exhibits. Twenty‐five exhibits out of the 105 contained both sildenafil and tadalafil. The contents of sildenafil ranged from 4.3 to 453.2 mg; for tadalafil, the range was 2.2–40.4 mg. The proportion of cases of having more than 100 mg of sildenafil was 50% and 78% had more than 20 mg of tadalafil. 相似文献
99.
目的 :建立反相高效液相色谱法检测槲皮素胶囊中槲皮素含量方法。方法 :采用Kromasil C18色谱柱 (4 .6mm× 2 5 0mm ,粒径 5 μm ) ,甲醇 磷酸盐缓冲液 (10 0 0mlH2 O +4mlH3PO4 +2mlTEA) (60∶4 0 )为流动相 ,检测波长 373nm ,流速 1.0ml/min ,柱温 30℃。结果 :槲皮素与共存的杂质分离很好。槲皮素在 7~ 70 μg/ml范围内 ,浓度与峰面积呈线性关系,r =0 .9999。平均加样回收率为 99.4 7% ,RSD为 0 .97%。结论 :该方法简单、准确、快速、可靠 ,可作为槲皮素胶囊的质量控制标准。 相似文献
100.
目的:建立乐脉软胶囊中芍药苷的含量测定方法.方法:采用高效液相色谱法测定该药中芍药苷的含量,色谱条件:汉邦Lichrospher C 18 柱(250.0 mm×4.6 mm,5 μm),乙腈水冰醋酸(16∶84∶0.8)为流动相,检测波长230 nm,柱温25℃,流速0.8 ml/min.结果:芍药苷浓度为 7.75~ 124.00 μg/ml时峰面积与浓度线性关系良好, r =0.999 7,平均回收率为97.50%,RSD为 1.62%.结论:HPLC简便易行,准确可靠,专属性强,可用于乐脉软胶囊的质量控制. 相似文献