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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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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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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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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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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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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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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 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