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1.
用HPLC/ECD法测定血小板5-HT,运用 WatersμBondapak C柱,3,4二羟基苄胺(DH-BA)作内标,以 0.07 mol/L乙酸钠缓冲液+乙腈为流动相(20+1),每1L缓冲液含 0.05 mol/L柠檬酸、2.5 mmol/L庚烷磺酸钠、0.1mmol/L Na_2EDTA,流速0.8 mL/min。DHBA和 5-HT的保留时间分别为5.4和11.5 min,线性范围为0.025~1mg/L(r= 0.9997)。5-HT日内 RSD低于1.87%,日间RSD低于8.54%,方法回收率为100.4%±2.3%。提示本方法快速简便,灵敏准确,适用于临床基础研究。 相似文献
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液相色谱测定糙米中烯虫酯残留量 总被引:2,自引:0,他引:2
研究了液相色谱测定糙米中烯虫酯残留量的方法。试样用丙酮提取,经活性炭,中性氧化铝层析柱一步净化,用液相色谱测定。线性范围0.2-10.0mg/L,检出限为0.05mg/L,当添加浓度0.5-10.0mg/kg时,回收率为84.2%-100.7%之间。用于糙米中烯虫酯残留量检验,结果满意。 相似文献
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基于固定化酶的流动荧光法测定血清中的葡萄糖 总被引:5,自引:0,他引:5
本文将固定化酶柱,光纤以及停流技术结合起来,研究了以廉价而易得的硫胺素为荧光底物的葡萄糖的荧光分析,提出了一种快速、简便、精确地测定葡萄糖的新方法。其线性范围为1.0 ̄60.0mg/L,线性相关系数为0.999,检测限为0.15mg/L。以5.0mg/L的葡萄糖作精度试验,RSD%=2.1%(n=11)。该方法已成功地用于血清中葡萄糖的测定,结果与光度法相符。 相似文献
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用鲁米诺-双氧水-铬(Ⅲ)化学发光体系结合巯基棉对As(Ⅲ)的富集分离,建立了快速的测定化探样品中痕量砷的新方法,检测线性范围为1.0*10^-4-1.0*10^1mg/L,检出限为3.4*10^-5mg/L。用于实际化探样吕测定,相对标准偏差为5.5^-9.0%。 相似文献
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流动注射光化学荧光法测定药物制剂中的盐酸氯丙嗪 总被引:10,自引:3,他引:10
氯丙嗪的流动注射光化学反应在一编结反应器中进行,该反应器盘绕在一荧光灯上并接受由该灯发生出的最大幅波长为365nm的紫外线照射。用253.0nm的激发波长和374.5nm的荧光波长在线测定光化学反应产物的荧光强度。在最佳条件下,检测限为5.4μg/L,采样速度为90次/h,1mg/L的分析物11次测定的相对标准偏差为0.5%,动态线性范围为0.01-6.00mg/L。所建立的方法已成功地地用于片剂 相似文献
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研究了影响毛细管区带电泳激光诱导荧光间接检测环腺苷单磷酸和环鸟苷单磷酸的实验条件。cAMP和cGMP的线性范围分别为30 ̄500mg/L和15 ̄500mg/l,其最低检测限分别为9.0mg/L和0.5mg/L; 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