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1.
应用制备高效液相色谱同时制备6种大豆异黄酮单体的方法研究 总被引:1,自引:0,他引:1
经大孔吸附树脂纯化大豆异黄酮粗提物后,以制备型高效液相色谱法(PHPLC)分离得到高纯度的大豆异黄酮单体。以SHIM-pack PRC-ODS(20 mm×250 mm,5 μm)制备柱,考察了流动相组成及流速、进样量对分离度的影响,确定了最佳色谱条件为乙腈-水流动相梯度洗脱,进样量800 μL,流速10 mL/min,在120 min内实现了6种异黄酮单体的基线分离及制备。经超高效液相色谱-串联质谱(UPLC-MS/MS)鉴定,6种异黄酮单体依次为大豆苷、黄豆黄苷、染料木苷、大豆素、黄豆黄素、染料木素。6种产品的纯度分别为95.54%、90.14%、100%、100%、96.27%、100%。方法具有简便易行、稳定性好、产品纯度高等特点,适用于大豆异黄酮标准品的制备。 相似文献
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经大孔吸附树脂纯化大豆异黄酮粗提物后,以制备型高效液相色谱法(PHPLC)分离得到高纯度的大豆异黄酮单体。以SHIM-pack PRC-ODS(20 mm×250 mm,5μm)制备柱,考察了流动相组成及流速、进样量对分离度的影响,确定了最佳色谱条件为乙腈-水流动相梯度洗脱,进样量800μL,流速10 mL/min,在120 min内实现了6种异黄酮单体的基线分离及制备。经超高效液相色谱-串联质谱(UPLC-MS/MS)鉴定,6种异黄酮单体依次为大豆苷、黄豆黄苷、染料木苷、大豆素、黄豆黄素、染料木素。6种产品的纯度分别为95.54%、90.14%、100%、100%、96.27%、100%。方法具有简便易行、稳定性好、产品纯度高等特点,适用于大豆异黄酮标准品的制备。 相似文献
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用HPLC法测定了丰城鸡血藤中的大豆黄素、染料木黄酮、异甘草素、美皂异黄酮含量。鸡血藤中黄酮用80%乙醇溶液(含盐酸10%)提取水解。采用Symm etry C18柱,以0.1%磷酸-乙腈为流动相,梯度洗脱,流速0.8 mL.m in-1,紫外双波长检测:λ1=260 nm(大豆黄素、染料木黄酮、美皂异黄酮)和λ2=370 nm(异甘草素)。大豆黄素、染料木黄酮、异甘草素、美皂异黄酮线性范围分别为2.08~208 mg.L-1(r=0.999 9)、0.96~96 mg.L-1(r=0.999 9)、1.12~44.8 mg.L-1(r=0.999 9)、1.16~116 mg.L-1(r=0.999 9),回收率在92%~103%之间,RSD(n=4)为0.75%~4.69%。实验结果表明该法快速、简便、准确可靠。 相似文献
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建立超高效液相色谱法同时测定淡豆豉配方颗粒中3种异黄酮(大豆苷元、黄豆黄素、染料木素)的含量。选择Eclipse Plus C18 RRHD色谱柱(100 mm×2.1 mm,1.8μm),流动相为乙腈-0.1%乙酸溶液,梯度洗脱,流量为0.3mL/min,柱温为30℃,检测波长为260 nm。大豆苷元、黄豆黄素、染料木素的质量浓度分别在18.41~184.14、0.48~4.82、30.65~306.46μg/mL范围内线性关系良好(r≥0.999 9)。样品测定结果的相对标准偏差分别为1.80%、2.20%、1.71%(n=6),平均加标回收率分别为96.49%、100.93%、98.53%。该方法快速,准确、可靠,可为淡豆豉配方颗粒的质量控制提供参考。 相似文献
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高效液相色谱法测定保健食品中的大豆异黄酮 总被引:5,自引:0,他引:5
建立了一种测定保健食品中大豆异黄酮的高效液相色谱分析方法,该方法可以使常见的大豆异黄酮6种主要成分大豆甙、黄豆甙、染料木甙、大豆甙元、黄豆黄素、染料木素得以分离和检测。采用乙腈-磷酸水溶液(pH2.8)作流动相,梯度洗脱,Venusil MP-C18色谱柱(150 mm×4.6 mmi.d.,5μm),流速为1.0 mL/min,紫外检测器,检测波长254 nm。结果表明各组分线性关系良好,相关系数R2为0.9991~0.9998,加标回收率在87%~106.9%,相对标准偏差均小于2%。检出限0.25~0.48μg/mL,该方法可同时测定大豆异黄酮的6种成分。 相似文献
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采用反相高效液相色谱法(RP-HPLC),以磺丁基醚-β-环糊精(SBE-β-CD)作为手性流动相添加剂,建立了二氢黄豆苷原(dihydrodaidzein)、雌马酚(equol)和山姜素(alpinetin)3种黄酮类化合物的手性拆分方法。考察了环糊精的种类和浓度、有机相的种类和比例、缓冲盐的种类和浓度以及pH对3种化合物手性拆分效果的影响。结果表明:采用Kromasil 100-5C18(250 mm×4.6 mm, 5 μm)色谱柱,流动相为乙腈-10 mmol/L SBE-β-CD水溶液(含20 mmol/L KH2PO4, pH值到4.0)(体积比为20:80)的条件下,二氢黄豆苷原、雌马酚和山姜素的对映体都达到了基线分离,分离度分别为1.8, 1.9和1.4。该方法简便,分离效果好,对黄酮类化合物的拆分具有应用价值。 相似文献
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建立了反相高效液相色谱测定异黄酮甙元的方法。采用Hypersil BDS C18色谱柱(250×4.6 mm i.d.,5μm),流动相为甲醇(A)、0.5%乙酸水溶液(B),流速为1.0mL/min,柱温为35℃,检测波长为260 nm,进样量为10μL。结果表明:大豆黄素的线性范围为0.0450~0.3150μg,加标回收率为99.05%,相对标准偏差(RSD)为1.31%;染料木黄酮的线性范围为0.0448~0.3136μg,加标回收率为98.82%,RSD为0.50%。方法可用于豆豉及其它大豆制品中异黄酮甙元的测定。 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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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