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毛细管电泳-电化学发光/电化学检测法同时测定维生素B_1和B_6 总被引:1,自引:0,他引:1
《分析科学学报》2015,(5)
建立了毛细管电泳-电化学发光/电化学检测(CE-ECL/EC)法同时测定维生素B1(VB1)和维生素B6(VB6)的新方法。在碱性条件下对VB1进行水解,可增强其电化学发光信号,并采用序贯均匀设计对毛细管电泳分离条件进行优化,测定VB1的电化学发光信号和VB6的电化学信号。VB1和VB6能在5min内得到良好的分离。电化学发光强度与VB1浓度在5.0~5 000.0μg/mL范围内具有良好的线性关系(r=0.997),检测限(S/N=3)为2.7μg/mL;电流强度与VB6浓度在10.0~1 000.0μg/mL范围内具有良好的线性关系(r=0.998),检测限(S/N=3)为6.8μg/mL。VB1和VB6的加标回收率范围为96.0%~100.0%,相对标准偏差为1.4%~6.7%。用建立的方法对复合VB片中的VB1和VB6进行测定,结果较好。 相似文献
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PAN-Co配合物用于维生素B12的示波测定 总被引:5,自引:0,他引:5
维生素 B12 是一种用于治疗恶性贫血和其他巨细胞型贫血的药物 .对维生素 B12 的测定 ,一般采用光度法[1~ 4 ] ,通过测定维生素 B12 中的钴含量可以换算出维生素 B12 的含量 . 1 - ( 2 -吡啶偶氮 ) - 2 -萘酚( PAN)是一种萃取光度法和光度测定或荧光测定 Al3+、Cd2 +、Co2 +、Ga3+等金属离子的显色剂 .在适宜的 p H值条件下 ,PAN能与 Co2 +等多种金属离子形成有色配合物 [5] .本文利用 PAN可在 Na OH底液中产生灵敏切口且当向其中加入含 Co2 +的溶液时 ,PAN的切口随 Co2 +的加入量线性降低的示波特性 ,对维生素 B12 中的钴含量… 相似文献
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反相高效液相色谱-化学发光法测定复合维生素片剂中的维生素B1和B2 总被引:14,自引:0,他引:14
基于水溶性维生素在碱性介质中只有维生素B1(VB1)和维生素B2(VB2)可以被K3Fe(CN)6直接氧化产生化学发光的原理,建立了反相高效液相色谱(RP-HPLC)分离柱后化学发光检测VB1和VB2的新方法,并成功应用于复合维生素B片剂中VB1和VB2的测定。该方法测定VB1,VB2的线性范围分别为1.0×10-3~1.0 g/L和1.0×10-3~0.1 g/L,检出限分别为2×10-4 g/L和8×10-4 g/L。对1.0×10-2 g/L VB1,VB2溶液连续11次测定的相对标准偏差 相似文献
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紫外吸光光度法测定维生素B12 总被引:1,自引:0,他引:1
李姝 《理化检验(化学分册)》2005,41(1):53-54
维生素B12,学名Coα-[α-(5,6-二甲基苯并咪唑基)]-Coβ氰钴酰胺,广存于动植物体中,它与核酸、蛋氨酸的合成,甲基代谢及动物体内蛋白质、脂肪、碳水化合物的代谢有密切关系,是一种应用较广的维生素类药物,其测定方法有紫外吸光光度法、HPLC法、毛细管电泳法等。有报道引入表面活性剂OP可以提高测定VB1、VB2、VB6的灵敏度, 相似文献
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建立了一种双波长共振瑞利散射光谱测定维生素B12的新方法. 在pH=1.0的HCl介质中, 维生素B12(VB12)与12-钨磷酸(TP)形成摩尔比为3:1的离子缔合物, 导致双波长共振瑞利散射(DWO-RRS)、 二级散射(SOS)和倍频散射(FDS)光谱显著增强, 其最大散射波长分别位于330和370 nm(RRS), 608 nm(SOS)和386 nm(FDS). 在一定范围内, 3种散射增强(ΔIRRS, ΔISOS和ΔIFDS)均与VB12的浓度成线性关系. 该方法具有较高的灵敏度, RRS, SOS和FDS法对VB12的检出限(3σ)在2.0~7.6 ng/mL之间. 研究了反应条件和共存物质的影响, 结果表明, 该方法具有良好的选择性. 据此, 提出了简便、 快速、 准确且高灵敏测定痕量VB12的光散射新方法, 适用于片剂和尿样中VB12的测定. 还对反应机理和散射光谱增强的原因进行了讨论. 相似文献
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用循环伏安法制备了银掺杂聚L-精氨酸修饰玻碳电极(Ag-PLA/GCE),研究了修饰电极的电化学交流阻抗及维生素B2和维生素B12(Vb2)在Ag-PLA/GCE电极上电化学行为,分析了维生素B2(Vb12)的吸附特性,建立了同时测定Vb2和Vb12的新方法。阻抗图谱说明,由于Ag-PLA修饰,提高了电子传输速率。当Vb2和Vb12同时存在时,在pH 5.0的磷酸盐缓冲溶液中,采用差分脉冲伏安法(DPV法)进行扫描测定,Vb2和Vb12的氧化峰电位分别为-0.470 V和-0.880 V,两种维生素的峰电位差值为:ΔE=0.410 V,不需分离,可同时进行测定。同时测定Vb2和Vb12的线性范围分别为0.10~15.0μmol/L和0.75~12.5μmol/L,检出限分别为0.03μmol/L和0.5μmol/L。方法已用于复合维生素药片中维生素B2和维生素B12的测定。 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 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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A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL. 相似文献
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A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions. 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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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 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