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高效液相色谱法测定金银花中保卫田残留量 总被引:7,自引:0,他引:7
本文用高效液相色谱法测定金银花保卫田残留量,使用ODS柱,流动相2%,NH4Ac-甲醇(6:4),流速1mL/min柱温30℃紫外检测器检测波长285nm,方法加标回收率80.3%~89.3%方法最低检出浓度0.02μg/g。 相似文献
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本文采用双波长薄层扫描仪,以紫外吸收方式,测定了感冒通片中扑尔敏的含量,其测定波长λs=260nm,参比波长λR=320nm,所用薄层板为GF254,薄层厚度为0.4mm,展开剂为苯∶氯仿∶冰HAC∶甲醇=5∶5∶0.5∶0.6,回收率为101.6%。 相似文献
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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非洲刺李提取物中阿魏酸二十二烷酯 总被引:2,自引:0,他引:2
建立了非洲刺李提取物中阿魏酸二十二烷酯含量测定方法。采用SpherisorbC18柱,以甲醇为流动相,检测波长326nm,柱温40℃,线性范围10~100mg/L(r=0.9995)。平均回收率98.4%,RSD为1.98%。方法准确可靠,重现性好。 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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高效液相色谱法分析人血清中硫唑嘌呤和巯嘌呤的浓度 总被引:3,自引:0,他引:3
建立了用HPLC同时测定人血清中硫唑嘌呤(AZP)和6-巯基嘌呤(6-MP)浓度的方法。血清样品经乙腈除蛋白后在常压和37℃下用氮气吹干,残余物用100μL洗脱液溶解,离心后上清液直接进样。以SpherisorbC18固定相,采用梯度洗脱,从V(乙腈)∶V(0.01mol/L磷酸二氢钾)=3∶97经5min时变为18∶82,15min后再变为50∶50,检测波长开始为325nm,10min后为278nm,甲硝唑(MNZ)为内标。AZP和6-MP平均回收率分别为(100.6±4.2)%和(102.4±4.5 )%。 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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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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《Tetrahedron》2014,70(21):3377-3384
The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative. 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