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5-磺酸钠间苯二甲酸二甲酯的高效液相色谱法分析 总被引:2,自引:1,他引:1
提出了用离子对反相高效液相色谱分析5-磺酸钠间苯二甲酸二甲酯的方法,色谱柱为HypersilBDSC18,5μm,250mm×4.6mm,流动相为V(甲醇)∶V(水)=60∶40(甲醇中含四丁基磷酸二氢铵10mmol/L),柱温为30℃,流速为0.8mL/min,进样体积为20μL,检测波长为220nm。用外标法进行了定量,相对标准偏差和回收率分别为0.26%和98.1%~99.6%。 相似文献
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高效液相色谱法测定人血浆中甲磺酸培氟沙星浓度 总被引:5,自引:0,他引:5
建立了一种测定人血浆中甲磺酸培氟沙星的匠相液相色谱方法,用的是ZorbaxODSC_(18)柱和用三乙醇胺调节成pH为3.0的甲醇-0.04mol/LH_3PO_4溶液(80:20,V/V)的流动相,检测在276nm处进行,流量为1mL/min,线性范围是6.01×10 ̄(-8)~3.01×10 ̄(-5)mol/L(γ=0.9998),检测极限为6.01×10 ̄(-8)mol/L,平均回收率为97.57±3.04%,日内与日间的CV分别为3.29%和5.08%。 相似文献
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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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高效液相色谱法测定环境水中痕量4,4′-二氨基联苯、4-硝基酚和苯酚 总被引:2,自引:0,他引:2
采用PhenomenexSpherexC18色谱柱,以含50mmol/L乙酸-乙酸钠缓冲溶液(pH6.0)的V(乙腈)∶V(乙醚)∶V(水)=12∶10∶78混合溶液为流动相,用分光光度法检测,检测波长为275nm,在16min内实现了4,4′-二氨基联苯、4-硝基酚和苯酚的同时分离测定。检测限分别为0.14,0.19和0.08ng。标准回收率分别为98.85%,98.15%和98.10%。方法灵敏度高,用于环境水样分析时结果令人满意。 相似文献
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液相色谱法测定血浆中三环类抗忧郁药物 总被引:2,自引:0,他引:2
用高效液相色谱法测定了血浆中4种三环类抗忧郁药物:卡马西平、氯氮平、多虑平和阿米替林。方法采用C_(18)色谱柱分离,二极管阵列检测器检测,流动相为甲醇:0.5mol/L三乙胺-0.5mol/L冰醋酸的水溶液(90:10,V/V;pH7.5)。标准曲线的线性范围为0~10mg/L,相关系数在0.99以上。方法的最小检出浓度为10~40μg/L血浆。血中药物经溶剂萃取后,药物的回收率为73.67%~98.24%,血中杂质不影响药物的检测。方法简便、快速,适用于临床中毒样品的分析。 相似文献
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反相HPLC测定钒,铌,钽的2—(2—吡啶偶氮)—5—二乙氨基苯酚配合物 总被引:1,自引:0,他引:1
以2-(2-吡啶偶氮0-5-二乙氨基苯酚(PADAP)为柱前衍生试剂,在含0.1%酒石酸的10mmol/L(pH3.5)HAc-NaAc缓冲溶液的甲醇/水(50∶50,V/V)中(580nm检测),在C18柱上于11min内实现了V、Nb、Ta的同时分离及测定,检出限(S/N=3)杰0.34、0.29、7.30ng/mL.该法灵敏度高,用于矿样分析所得民推荐值相行,标准加入回收率为99.0%~10 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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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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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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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