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施介华 《分析测试技术与仪器》1999,5(3):151-154
采用气相色谱法分离和测定对甲硫苯酚。在Ф6 ×1 .5 ×1 500 m m 玻璃柱内填充5 % O V101/ Chrom osorb W A W D M C S 的色谱柱上,对甲硫基苯酚与内标物磷酸三丁酯及杂质之间具有较好的分离效果;而且以磷酸三丁酯为内标物时其重量校正因子相当稳定,即 fw . A = 0 .948 ±0 .005 4(n = 9 ,α= 0 .05) 。该方法操作简便、快速、准确。对同一试样的8 次平行独立测定其标准偏差为0 .25 ,变异系数为0 .007 2 。并且,该方法的3 次加入法回收率达98 .18 % ~99 .22 % 。 相似文献
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分光光度法研究血清蛋白质与钍试剂Ⅰ的作用 总被引:10,自引:0,他引:10
钍试剂Ⅰ是测定无机离子的显色剂,在pH 3.8 的Britton-Robinson缓冲溶液中,该试剂能与血清蛋白质形成复合物,λm ax为535 nm ,比试剂本身红移约55 nm ,表观摩尔吸光系数为3.56 ×105 L·m ol- 1·cm - 1(BSA),测定蛋白质的线性范围,为20~160 m g/L。用于人血清样品总蛋白的测定,RSD为1.05 % (n= 4),回收率约为100 % 。方法基本无干扰。 相似文献
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铁,钴,镍的反相高效液相色谱分离和测定 总被引:4,自引:0,他引:4
1引言建立了用反相高效液相色谱同时测定铁、钴、镍的分析方法并对Men+-二硫腙(DZ)体系的色谱行为进行了探索。较之萃取进样更快速、简便。测定条件为:Shim-PackCLC-ODS(φ6×150mm,5μm);流动相:甲醇:水:三氯甲烷(含1%三乙胺)(80:10:10);流速1mL/min;柱温35℃;检测波长254n。线性范围0.01-2.0mg/L;相关系数r=0.999l~0.9998;检测限为0.0023~0.0050mg/L;相对标准偏差为1.8%-2.7%;回收率为96%-104… 相似文献
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聚氯乙烯膜奎宁选择电极的研制与应用 总被引:4,自引:0,他引:4
本报道了一种以奎宁溴汞酸盐为电活性物的PVC膜奎宁选择电极,其线性响应范围为1.0×10^-2-1.0×10^-6mol/L;级差58±1mV;检测限为8.2×10^-7mol/L。以此电极测定奎宁的含量,方法简单、快速、结果与药典法相符。 相似文献
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离子色谱法测定α—氧化铝中微量硫酸根的研究 总被引:1,自引:0,他引:1
本建立了用氢氧化钠溶样,离子色谱测定α-Al2O3中微量硫酸根的方法。在DionexAS4A分离柱上,用1.8×10^-^3mol/LAa2CO3作流动相进行洗脱,电导检测器检测,分析方法简便,快速,硫酸根的检测限为1.0×10^-^2μg/ml,相对标准偏差为2.67%,回收率为97.5%,扩展了离子色谱法测定实际样品的范围。 相似文献
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用动态涂敷法制备了对甲苯磺酸正丁铵玻璃毛细管柱柱1(固定液浓度为7.5%,柱尺寸为35m×0.35mmi.d.)和柱2(固定液浓度为9.2%,柱尺寸为35m×0.30mmi.d.),所用溶剂是丙酮和甲醇(2:1V/V)的混合溶剂,并对柱性能进行了考察。结果表明,这种色谱固定相具有较强的极性并对饱和烃、芳香烃、饱和酸、芳香酸、极性异构体等具有良好的分离效果。 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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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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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
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Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described. 相似文献
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用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在. 相似文献
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Jona Mirnik Eva Pušavec Kirar Sebastijan Ričko Uroš Grošelj Amalija Golobič Franc Požgan Bogdan Štefane Jurij Svete 《Tetrahedron》2017,73(24):3329-3337
A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu0 as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than CuI in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT). 相似文献
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George E. Magoulas Thomas Garnelis Constantinos M. Athanassopoulos Dionissios Papaioannou George Mattheolabakis Konstantinos Avgoustakis Dimitra Hadjipavlou-Litina 《Tetrahedron》2012,68(35):7041-7049
(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C60, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine. 相似文献