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高效液相色谱法测定血浆中表阿霉素浓度 总被引:3,自引:0,他引:3
报道了高效液相色谱法测定血浆中表阿霉素浓度的实验方法。采用μBondapakC_(18)色谱柱,正磷酸、甲醇、乙腈、异丙醇为流动相。荧光检测器检测,激发波长为450nm,发射波长为530nm。血浆经离心后,取血清,用甲醇沉淀蛋白。方法的平均相对回收率为99.4%±4.6%,日内和日间平均RSD小于5%和6%。最低检测限为3ng。本方法快速、准确,灵敏度高。 相似文献
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花生中黄曲霉毒素B1、B2、G1、G2的多功能净化柱-高效薄层色谱分析 总被引:1,自引:0,他引:1
建立了一种测定食品中黄曲霉毒素( AFT) B1 、B2 、G1 、G2 的多功能净化柱( MFC) 净化, 单相展开的薄层色谱法。 以乙腈- 水( 体积比9 ∶1) 提取样品中AFT, 经MFC 净化浓缩后, 采用HSG60 薄层板, 以丙酮- 氯仿( 体积比9 ∶1) 展开, 薄层扫描仪荧光检测扫描定量。该法用于花生样品的检测,4 种毒素的分离良好; 线性范围:0 .05 ~1 .0 ng, 相关系数≥0 .999 1; 检出限均达到0 .5 ×10 - 9 ; 相对标准偏差为4 .67 % ~10 .21 % ; 样品加标0.5 ×10 - 9 ~10 ×10 - 9 , 平均回收率为86 .5 % ~99 .0% 。 相似文献
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本文研究了快速、简便测定蜂皇浆及制品中添加的低含量维生素B_6的HPLC法。称取适量样品,用10%偏磷酸提取、净化,清液供HPLC分析用。WATERS荧光检测器,激发波长290nm,发射波长390nm,VB_6含量在0~120ng之间工作曲线相关系数大于0.999,样品中VB_6含量为0.1%~5%时,方法回收率为92.17%~98.42%,相对标准偏差(n=6)小于3.7%。 相似文献
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贵金属冶金物料中微量钯、铂、铑的双波长分光光度法同时测定的研究 总被引:2,自引:0,他引:2
本文提出了用二苄基二硫代乙二酰胺(DbDO)为显色剂分光光度测定铑的方法,并进一步研究了该试剂与钯、铂的反应,从而建立了可在一个试样中同时测定该三元素的方法。在2~3mol/LHC1溶液中,钯与DbDO在室温显色,用氯仿萃取并用8.4mol/LHC1振荡有机相,然后在454nm测定。在萃余液中加入SnCl_2,并在沸水浴中加热,使铂、铑的DbDO络合物生成,再用氯仿萃取,8.4mol/LHC1振荡有机相,以双波长分光光度法同时测定。其中铂用双波长系数倍率法(λ′_2=521nm,λ′_1=500nm,K=2.563),铑用双波长等吸收波长法(λ_2=400nm,λ_1=546nm)。铂和铑的含量为1:5或5:1时互不干扰。 相似文献
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用免疫亲和柱分离、高效液相色谱法测定花生和玉米中黄曲霉毒素的研究 总被引:5,自引:0,他引:5
建立了用免疫亲和柱分离净化、高效液相色谱法测定花生和玉米中黄曲霉毒素(AFT)B_1、B_2、G_1、G_2的方法。采用60%甲醇提取样品中的AFT,氢氧化铁沉淀吸附除去样品液中大部分杂质,再经过亲和柱将AFT截留,进一步与杂质分离,洗脱后,加三氟乙酸衍生化处理,反相高效液相色谱法分离定量。对样品中四种AFT的最低可测下限浓度均为1μg/kg,样品加标5~10μg/kgAFT,回收率在76.9%~113.6%范围内。 相似文献
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采用免疫亲和层析柱吸附食品样品中的黄曲霉毒素B1,以荧光色谱-柱后光化学衍生法测定食品中黄曲霉毒素B1的含量。样品用甲醇-水溶液(体积比为7:3)混合,均质器高速搅拌提取,经免疫亲和层析柱纯化后,通过LachromC18色谱柱进行分离,以甲醇一水溶液(体积比为45:55)作为流动相,荧光检测器激发波长为360nm、发射波长为420nm,外标法定量。黄曲霉毒素B,的质量浓度在1~20ng/mL范围内与色谱峰面积线性关系良好,相关系数r=0.9998,检出限为0.1gg/kg。在3个添加水平下,样品的加标回收率在88.5%~97.9%之间,相对标准偏差均小于3%(n=6)。该方法操作简单、定量准确,可用于食品中黄曲霉毒素B.的定量定性检验。 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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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 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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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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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 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