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讨论了用CAS-CPB胶束增溶比色法测定头发中铝含量的最佳实验条件,最大吸收波长为630nm,铝的线性范围为0 ̄4.0μg,变异系数CV=3.2%(n=6),回收率为98%。 相似文献
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铜(Ⅰ)—苯骈三氮唑络合吸附波的极谱研究与应用 总被引:4,自引:0,他引:4
本文在0.6mol/L NH3-NH4Cl缓冲溶液(pH=9.8)中,Cu(Ⅱ)在滴汞电极上还原生成Cu(Ⅰ),可与苯骈三氮唑(BTA)络合,产生一灵敏的络合吸附波,Ep=-0.73V(us,SCE)。苯骈三氮唑的浓度在0.40-10.0mg/L范围内与极谱波峰高呈线性关系,检测下限为0.40mg/L,相对标准偏差为1.4%-3.2%;回收率为97.5%-101.5%。 相似文献
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本文采用二阶导数光谱法,测定呋麻滴鼻液中盐酸麻黄碱的含量,排除了呋喃西林的干扰,方法简单,快速,准确。平均回收率为99.5%(n=8),SD=0.73,CV=0.73%。\ 相似文献
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研究了以PAN为指示剂,硫酸铜为回滴剂的EDTA络量法测定铝的终点判别的影响因素,并根据试验中所接触到样品组成不同、铝量及干扰离子不同等条件,对终点的影响作了进一步探讨,得出终点判断依据为EDTA:Cu^2+:Al^3+之间的摩尔比为1:(0.2~0.3):(0.7~0.8)之间,且服从nEDTA=nCu+nAl。 相似文献
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注射用舒尔哌酮的高效液相色谱分析 总被引:1,自引:0,他引:1
建立了高效液相色谱法分离与测定复方制剂舒尔哌酮中斯巴坦及头孢哌酮的含量。采用C_(18),10μm,4.6mm×250mm(大连化物所Spherisorb)柱,以0.25%三乙胺溶液(用磷酸调pH6.0)+乙腈(86.5+13.5)为流动相,在紫外检测器210nm波长处进行检测,线性范围0.05~0.6mg/mL,γ=0.9999(n=5),精密度:斯巴坦及头孢哌酮的日内平均RSD分别为0.6%及0.75%(n=18),日间平均RSD分别为0.86%及0.87%(n=12)。 相似文献
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反相合并带流动注射分析法测定维生素C的含量 总被引:2,自引:0,他引:2
采用流动注射反相合并带技术,在乙酸介质中,维生素C与过量的I3反应,剩余的I3在350nm处由检测器检出,信号强度△A与维生素C含量在0~5.0×10^-5mol.L^-1范围内呈良好的线性关系,相关系数r=0.9995,相对标准偏差RSD=0.4%(n=11),采样频率为70次次/h。 相似文献
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烟草中Fe,Co一阶导数分光光度法同时测定的研究 总被引:4,自引:0,他引:4
本文研究了在pH4.0时,meso-四(4-磺酸基苯基)卟啉与铁、钴同时络合显色的反应条件以及一阶导数光谱行为。此体系一阶导数的灵敏度比零阶导数灵敏度高。Fe ̄(3+)~0.18μg/mL、Co ̄(2+)0~0.24μg/ml,范围内符合比耳定律;检测限为:Fe ̄(3+)=0.48ng/mL,Co ̄(2+)=0.2ng/mL。回收率为:Fe98.5%~100.8%,Co99.2%~101.3%。此方法用于烟草中痕量Fe、Co测定,与AAS值相比较,结果令人满意。 相似文献
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An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions. 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
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An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction. 相似文献
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The Diels-Alder reactivity of 1,2-heteroborines (H4C4B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed. 相似文献
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Xi-Liu YunWen-Ying Bi Jian-Hui HuangYu Liu Daisy Zhang-NegrerieYun-Fei Du Kang Zhao 《Tetrahedron letters》2012,53(38):5076-5080
A variety of N-aryl and N-alkyl carbazolones were conveniently achieved in good to high yields via Pd2(dba)3-mediated intramolecular coupling of N-substituted α-iodo enaminones under microwave irradiation. The Pd(0)-catalyzed cyclization was found to proceed favorably with the more electron-deficient phenyl ring during the reactions involving unsymmetrical N,N-diaryl α-iodo enaminones. This unique property enables the construction of carbazolone skeleton containing nitro substituted benzenoid ring. 相似文献
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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
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Both substituted 2,4,5,6-tetrahydrocyclopenta[c]pyrazoles and 2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazoles have been synthesized by the 3+2 intramolecular dipolar cycloaddition of nitrilimines to alkynes. This cyclization has been extended to more versatile 3-bromo derivatives by the use of alkynylbromides as dipolarophiles. 相似文献
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In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献