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11.
Simultaneous detection with a 700-A Hall? and an NPD detector is an effective technique for characterizing chloro-and chloronitroanilines in highly complex Publicly Owned Water Treatment Works (POTW) sludges. The utilization of a modified Varian effluent splitter and a SE-54 fused silica capillary column permitted the detection of mid-picogram quantities of the polar chloroanilines without sacrificing peak shape. The response of the Hall? detector in the halogen mode was roughly proportional to the number of chlorine atoms present, while the response of the Hall? in the nitrogen mode and the NPD was less predictably influenced by the presence of one or more nitro groups. When combined with retention time data, the ratio of the NPD response to the Hall? response has been found to substantiate the presence of chloro- and chloronitroanilines in sludge extracts. 相似文献
12.
痕量砷流动注射在线还原氢化物发生原子吸收测定 总被引:5,自引:0,他引:5
方法采用流动注射停流技术使水及土壤浸出液中As(V)在线还原为As(Ⅲ),不经手工还原,用氢化物发生原子吸收光谱法直接测定砷的含量。含4mol/L HCl的样品溶液与30%碘化钾溶液在编结式反应器中混合,并在采样环中停流40s,达完全还原后注入到载流中与硼氢化钠反应,采样速度55次/h,检出限(3δ)0.1μg/L,对自来水和土壤浸出液的加标回收结果满意。 相似文献
13.
A capillary electrophoretic assay for determining aloe-emodin (AE), methyl p-coumarate (MC), and 3,4-dihydro-6,8-dihydroxyl-[(3s)-2'-acetyl-3'-hydroxyl-5'-methoxy-benzyl]-isocoumarin (DDI) in Aloe vera has been developed. Baseline separation was achieved within 15 min using a running buffer of 20 mm borax containing 10% (v/v) acetonitrile at pH 10.5. A linear relationship between the peak area and the concentration of the analytes was found in the ranges 5-500, 10-1000 and 2-1000 micro g/mL for AE, MC and DDI, respectively, with correlation coefficients of 0.9992-0.9998. The relative standard deviations of migration time and peak area were within 0.17-0.19 and 1.52-3.37%, respectively. The recoveries of AE, MC and DDI were 105, 102 and 96.4%. The contents of AE, MC and DDI in Aloe vera were measured to be 5.13, 0.768 and 1.30 mg/g, respectively. 相似文献
14.
B. Kaufmann S. Souverain S. Cherkaoui P. Christen J. -L. Veuthey 《Chromatographia》2002,56(3-4):137-141
Summary A rapid analytical method has been developed for the mutual resolution of three steroidal compounds, withaferin A, iochromolide,
and withacnistin. Liquid chromatography was performed on a Chromolith analytical column (4.6 mm i.d.×50 mm), made from a cylindrical
silica rod, operated at a flow rate of 4 mL min−1 with a simple linear gradient prepared from 0.1% aqueous formic acid and 0.1% formic acid in acetonitrile. Under optimum
conditions simultaneous separation of the compounds was achieved in less than 7 min, one eighth the time required for conventional
LC separation. The overall analysis time was reduced without sacrificing chromatographic performance—essential for the resolution
of positional isomers such as iochromolide and withacnistin. The column was coupled to a single-quadrupole mass spectrometer
and the method was characterized by good performance in terms of repeatability, selectivity, linearity, and sensitivity. Detection
limits in the single-ion-monitoring mode were 0.15 μg mL−1 or below. Finally, the developed method was successfully applied to the determination of withanolides in extracts fromlochroma gesnerioides obtained by three different processes—traditional Soxhlet extraction and two faster methods, microwave-assisted extraction
and pressurized solvent extraction. 相似文献
15.
The polyphenolic profiles and antioxidant effects of Agastache rugosa Kuntze (Banga) flower,leaf, stem and root
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Yun‐Hi Kim Won Sup Lee Soo Jung Lee Jong Sung Jin A. M. Abd El‐Aty Ho‐Chul Shin Jae‐Han Shim Sung Chul Shin 《Biomedical chromatography : BMC》2016,30(2):225-231
Agastache rugosa Kuntze (Korean mint) is used as a spice and in folk medicine in East Asia. The present study identified a total of 18 polyphenols from the flower, leaf, stem and roots of this plant using high‐performance liquid chromatography–tandem mass spectrometry. Fourteen of these compounds had not previously been identified in these plant tissues. Each polyphenol was validated in comparison with external calibration curves constructed using structurally related compounds, with determination coefficients >0.9993. The limits of detection and quantification were 0.092–0.650 and 0.307–2.167 mg/L, respectively. Recoveries of 61.92–116.44% were observed at two spiking levels, with 0.91–11% precision, expressed as relative standard deviation (except anthraquinone spiked at 10 mg/L). Hydroxycinnamic acid was the most abundant compound in the root, while the flowers showed the highest total flavonoid level. Antioxidant activities, determined in terms of reducing power, Fe2+ chelating activity and the radical scavenging activities using α,α‐diphenyl‐β‐picrylhydrazyl and 2‐2?‐azino‐bis‐3‐ethylbenzothiazoline‐6‐sulfonic acid, increased in a concentration‐dependent manner; the highest activity was identified in the stems, followed by leaves > flowers > roots. These findings indicate that A. rugosa is a good source of bioactive compounds and can be used as a functional food. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
16.
Chia-Chi Huang 《应用光谱学评论》2016,51(1):1-11
Raman spectroscopic techniques are a group of chemical fingerprint detection methods based on molecular vibrational spectroscopy. They are compatible with aqueous solutions and are time saving, nondestructive, and highly informative. With complementary and alternative medicine (CAM) becoming increasingly popular, more people are consuming natural herbal medicines. Thus, chemical fingerprints of herbal medicines are investigated to determine the content of these products. In this study, I review the different types of Raman spectroscopic techniques used in fingerprinting herbal medicines, including dispersive Raman spectroscopy, resonance Raman spectroscopy, Fourier transform (FT)–Raman spectroscopy, surface-enhanced Raman scattering (SERS) spectroscopy, and confocal/microscopic Raman spectroscopy. Lab-grade Raman spectroscopy instruments help detect the chemical components of herbal medicines effectively and accurately without the need for complicated separation and extraction procedures. In addition, portable Raman spectroscopy instruments could be used to monitor the health and safety compliance of herbal products in the consumer market. 相似文献
17.
《Journal of separation science》2018,41(9):1938-1946
A new method has been developed for the simultaneous determination of 13 tropane alkaloids in tea and herbal teas using high‐performance liquid chromatography coupled to an Exactive‐Orbitrap analyzer. A mixture of methanol, water, and formic acid was used for the extraction of the target compounds followed by a solid‐phase extraction step. The validated method provided recoveries from 75 to 128% with intra‐ and interday precision lower than or equal to 24% (except for apoatropine). Limits of quantification ranged from 5 to 20 μg/kg. Eleven tea and herbal tea samples and two contaminated samples with Datura stramonium seeds were analyzed. Tropane alkaloids were detected in six samples with concentrations from 5 (apoatropine) to 4340 μg/kg (sum of physoperuvine, pseudotropine, and tropine), whereas concentrations from 5 (apoatropine) to 1725 μg/kg (sum of physoperuvine, pseudotropine, and tropine) were found in the contaminated samples. 相似文献
18.
19.
Strategies for differentiation of isobaric flavonoids using liquid chromatography coupled to electrospray ionization mass spectrometry
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Flavonoids are a class of secondary plant metabolites existing in great variety in nature. Due to this variety, identification can be difficult, especially as overlapping compounds in both chromatographic separations and mass spectrometric detection are common. Methods for distinguishing isobaric flavonoids using MS2 and MS3 have been developed. Chromatographic separation of various plant extracts was done with RP‐HPLC and detected with positive ESI‐MS operated in information‐dependent acquisition (IDA) mode. Two methods for the determination of flavonoid identity and substitution pattern, both featuring IDA criteria, were used together with the HPLC equipment. A third method where the collision energy was ramped utilized direct infusion. With the developed strategies, it is possible to differentiate between many isobaric flavonoids. Various classes of flavonoids were found in all of the plant extracts, in the red onion extract 45 components were detected and for 29 of them the aglycone was characterized, while the substituents were tentatively identified for 31 of them. For the strawberry extract, those numbers were 66, 30 and 60, and for the cherry extract 99, 56 and 71. The great variety of flavonoids, several of them isobaric, found in each of the extracts highlights the need for reliable methods for flavonoid characterization. Methods capable of differentiating between most of the isobars analyzed have been developed. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
20.