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1.
高效毛细管电泳-电导检测对四环素衍生物分离测定的研究 总被引:9,自引:0,他引:9
运用毛细管电泳-电导检测方法对4种四环素衍生物——土霉素(OTC)、金霉素(CTC)、强力霉素(DOC)和四环素(TC)的分离进行了研究。在3.5mmol/L三羟基氨基甲烷(Tris)-7.5mmol/L柠檬酸(Cit)pH4.0的运行缓冲液中,4种四环素衍生物在15min内获得完全分离。四环素衍生物的线性范围分别为5.0-500μg/mL OTC,3.6-420μg/mL CTC,4.5-470μg/mL DOC和2.5-400μg/mL TC。检测限(S/N=3)分别为OTC2.0μg/mL,CTC 1.8μg/mL,DOC2.5μg/mL和TC1.0μg/mL。采用本法对实际样品强力霉素片中强力霉素和土霉素片中土霉素进行测定,回收率分别为97.2%和96.4%。 相似文献
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火焰原子吸收光谱法连续测定菠萝中的铜、锌、铁、锰 总被引:6,自引:0,他引:6
探讨了用微波消化罐消化样品、以火焰原子吸收光谱法在同一体系中测定菠萝中微量元素铜、锌、铁、锰的方法。考察了硝酸、过氧化氢的不同用量以及消化时间长短的影响和在同一体系中钢、锌、铁、锰的彼此干扰情况。在选定条件下,检测限铜为0.0060μg/mL、锌为0.0074μg/mL、铁为0.0040μg/mL、锰为0.0090μg/mL,相对标准偏差1.9%-4.7%,回收率93.2%-105%。 相似文献
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DNA荧光探针—荧光素-中性红体系的研究 总被引:5,自引:0,他引:5
基于DNA对荧光素(FL)-中性红(NR)分子间荧光能量转移的抑制作用,以荧光素-中性红为荧光探针,考察该探针与DNA的结合反应,建立了准确测定DNA的新方法,在pH=6.5条件下,hsDNA、ctDNA和smDNA的浓度与荧光素-中性红体系的荧光比值变化量Δ(Fd/Fa)成线性关系,响应线性范围分别为0.25-6.25μg/mL、0.10-5.00μg/mL、0.10-4.00μg/mL,0.025μg/mL和0.023μg/mL;分析测定了DNA合成样品,回收率91.3%-101.4%,相对标准偏差小于4.2%. 相似文献
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在线还原富集火焰原子吸收光谱法测定环境水样中Cr(Ⅲ)和Cr(Ⅵ)的形态 总被引:2,自引:0,他引:2
采用单阀双阳离子交换树脂微柱并联,设计了双路采样逆向洗脱在线分离富集系统,该系统与原子吸收测量技术相结合,实现了在线分离富集-火焰原子吸收光谱法同时测定水中Cr(Ⅲ)和Cr(Ⅵ),富集1min时,分析速度为60样/h,测定Cr(Ⅲ)和Cr(Ⅵ)的特征浓度分别为6.08μg/L和11.58μg/L(相当于1%吸收),线性范围分别为0~1.0μg/mL和0~2.0μg/mL,对质量浓度为100μg/L的Cr(Ⅲ)和Cr(Ⅵ)测定的相对标准偏差分别为2.9%和3.0%、检出限分别为8.70和10.8μg/L。该法对实际水样加标回收率在94.5%~104.3%之间。 相似文献
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高效毛细管电泳电导法快速检测复方维生素B片中的VBl、VBl2、VB6和VC 总被引:1,自引:0,他引:1
采用高效毛细管电泳电导法同时分离、测定了复方维生素B片中的主要成分VB1,VB12,VB6和VC的含量。研究了运行缓冲溶液的酸度和浓度、电泳电压、进样时间等因素对电泳的影响。在优化的实验条件下:40mmol/L Tris-4mmol/L H3BO3(pH8.0)的缓冲溶液中加入0.30mmol/L CTAB(溴化十六烷基三甲基铵),分离电压为15kV,上述4组分在5min内得到良好的分离。维生素B1,B12,B6和VC的线性范围分别为5.5~1.0mg/mL;15~1.5mg/mL;1.0~0.40mg/mL和6.6~0.80mg/mL;检测限分别为0.80μg/mL,4.0μg/mL,0.50μg/mL,2.9μg/mL;5次测定峰高的相对标准偏差分别为2.2%,1.6%,3.9%,2.8%。5次测定的平均回收率分别为99%,94%,l00%,97%。 相似文献
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王铎 《广东微量元素科学》2005,12(9):64-66
研究了香蕉中的金属元素的含量和火焰原子吸收光谱法在同一体系中测定香蕉中微量元素铜、铁、锌、锰的方法,考察了硝酸、过氧化氢的不同用量以及消化时间长短的影响和在同一体系中铜、铁、锌、锰的相互干扰情况。在选定条件下铜检测限为0.064μg/mL,铁为0.275μg/mL,锌为0.157μg/mL,锰为0.187μg/mL,相对标准偏差为1.9%-4.7%,回收率为92.3%-105.0%。 相似文献
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建立了氯化亚锡还原-硫氰酸铵快速光度法测定合金钢中钨的方法,方法的线性范围为2-400μg/50mL,相对标准偏差为0.24%-1.22%,方法简便,快速,测定结果准确。 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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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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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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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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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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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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Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 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