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171.
Xin-Bo Zhou Jian-Rong Zhu Ji-Yong Liu Zhi-Ping Jin Fei-Yu Tang Xiu-Rong Hu 《Acta Crystallographica. Section C, Structural Chemistry》2019,75(5):545-553
Ivabradine hydrochloride (IVA‐HCl) (systematic name: {[3,4‐dimethoxybicyclo[4.2.0]octa‐1(6),2,4‐trien‐7‐yl]methyl}[3‐(7,8‐dimethoxy‐2‐oxo‐2,3,4,5‐tetrahydro‐1H‐3‐benzazepin‐3‐yl)propyl]methylazanium), is a novel medication used for the symptomatic management of stable angina pectoris. In many recent patents, it has been claimed to exist in a very large number of polymorphic, hydrated and solvated phases, although no detailed analysis of the structural features of these forms has been published to date. Here, we have successfully crystallized the tetrahydrate form of IVA‐HCl (form β), C27H37N2O5+·Cl?·4H2O, and elucidated its structure for the first time. Simultaneously, a new crystal form of IVA‐HCl, i.e. the hemihydrate (form II), C27H37N2O5+·Cl?·0.5H2O, was discovered. Its crystal structure was also accurately determined and compared to that of the tetrahydrate form. While the tetrahydrate form of IVA‐HCl crystallized in the orthorhombic space group P212121, the new form (hemihydrate) was solved in the monoclinic space group P21. Detailed conformational and packing comparisons between the two forms have allowed us to understand the role of water in the crystal assembly of this hydrochloride salt. The stabilities of the two forms were compared theoretically by calculating the binding energy of the water in the crystal lattice using differential scanning calorimetry (DSC). The stability experiments show that the tetrahydrate is stable under high‐humidity conditions, while the hemihydrate is stable under high‐temperature conditions. 相似文献
172.
采用超高效液相色谱-串联质谱(UHPLC-MS/MS)技术,建立了快速、简单、灵敏的测定人血浆中盐酸氨溴索含量的方法,并用于盐酸氨溴索人体生物等效性预试验研究。取50 μL血浆样品,采用蛋白沉淀法处理,以盐酸氨溴索-d5为内标。采用Waters XBridge BEH C18色谱柱(50 mm×2.1 mm,2.5 μm),以0.1%(v/v)甲酸水-含0.1%(v/v)甲酸的甲醇为流动相,在0.4 mL/min流速下进行梯度洗脱。采用电喷雾电离(ESI)源以正离子模式进行MRM检测。结果显示,盐酸氨溴索在2~400 ng/mL范围内线性关系良好,相关系数(r)为0.998,准确度为97.1%~108.7%,精密度为1.0%~5.6%。将该方法用于6名健康受试者口服盐酸氨溴索受试制剂和参比制剂30 mg后血药浓度的测定,结果显示二者相对生物利用度为(102.3±14.8)%,血药浓度-时间曲线下面积(AUC0-t、AUC0-∞)和最大血药浓度(Cmax)的90%置信区间均在80.0%~125.0%范围内,两种制剂生物等效。 相似文献
173.
Qi Chen Qian‐Yi Cheng Yan‐Chao Zhao Bao‐Hang Han 《Macromolecular rapid communications》2009,30(19):1651-1655
Novel glucosamine hydrochloride functionalized water‐soluble conjugated polyfluorene was easily synthesized through Cu(I)‐catalyzed azide/alkyne “click” ligation and Suzuki coupling polymerization. The water‐solubility and biocompatibility of the polymer were improved after grafting glucosamine hydrochloride to the side chains of the conjugated polymer. As a fluorescent model system of chitosan, its interaction with single‐stranded DNA was studied by spectrofluorometric titration.
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176.
In the present paper, the electronic band structure, density of states (DOS), and projected density of states (PDOS) analysis of thiocarbamide hydrochloride are reported. Calculations of the electronic properties have been carried out on the basis of fully self-consistent pseudopotential method using DFT. The results show that near the Fermi level, more prominent densities of states are seen between -8 eV and -6 eV in the valence band mainly due to the Cl-3p, N-2p and S-3p orbitals. 相似文献
177.
流动注射光度法测定药物中的盐酸氯丙嗪 总被引:1,自引:0,他引:1
在pH 4.04的HAc-NaAc缓冲液中, 刚果红与盐酸氯丙嗪在室温下迅速结合生成缔合物, 且缔合物在480 nm处有最大吸收. 基于此建立了流动注射光度法测定药物中盐酸氯丙嗪的含量. 方法线性范围为0.25~50.0 μg/mL, 检出限为0.082 μg/mL, 测定频率达80次/h. 相似文献
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179.
A simple isocratic reversed-phase high-performance liquid chromatographic method (RP-HPLC) was developed for the simultaneous determination of buprenorphine hydrochloride, naloxone hydrochloride dihydrate and its major impurity, noroxymorphone, in pharmaceutical tablets. The chromatographic separation was achieved with 10 mmol L−1 potassium phosphate buffer adjusted to pH 6.0 with orthophosphoric acid and acetonitrile (17:83, v/v) as mobile phase, a C-18 column, Perfectsil Target ODS3 (150 mm × 4.6 mm i.d., 5 μm) kept at 35 °C and UV detection at 210 nm. The compounds were eluted isocratically at a flow rate of 1.0 mL min−1. The average retention times for naloxone, noroxymorphone and buprenorphine were 2.4, 3.8 and 8.1 min, respectively. The method was validated according to the ICH guidelines. The validation characteristics included accuracy, precision, linearity, range, specificity, limit of quantitation and robustness. The calibration curves were linear (r > 0.996) over the concentration range 0.22-220 μg mL−1 for buprenorphine hydrochloride and 0.1-100 μg mL−1 for naloxone hydrochloride dihydrate and noroxymorphone. The recoveries for all three compounds were above 96%. No spectral or chromatographic interferences from the tablet excipients were found. This method is rapid and simple, does not require any sample preparation and is suitable for routine quality control analyses. 相似文献
180.
Detection of drug vapors and volatile products of their decomposition is an important, and sometimes the only way to determine the presence of illegal drug traces at the surface of mail items, documents, hands and banknotes. This paper gives the results of experimental studies on the effect of UV irradiation on the sensitivity of a vapor phase detection of cocaine of different origin by a technology of ion mobility increment spectrometry (IMIS). It is shown that the influence of UV irradiation on the surface of cocaine hydrochloride and crack increases the amplitude of IMIS signals by about eight times. We analyzed ions emerged by photolysis of tested cocaine samples using mass-spectrometry with atmospheric pressure ionization (API-MS). The assumption is made about structural formula of volatile products of photolysis of crack and cocaine hydrochloride. By the results of API-MS and IMIS studies on photolysis of cocaine samples it is assumed that compound C10H15NO3 with a molecular weight of 197 amu and ecgonidine methyl ester with a molecular weight of 181 amu are responsible for the increase of an amplitude of IMIS signals upon UV irradiation of samples of crack and cocaine hydrochloride. 相似文献