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高效液相色谱法同时测定参茸补酒中芍药苷、阿魏酸的含量 总被引:1,自引:0,他引:1
建立一种高效液相色谱双波长法同时测定参茸补酒中芍药苷、阿魏酸的含量。该方法采用Symmetry C18色谱柱(150×3.9mm,5μm),流动相为乙腈 水 冰乙酸(12∶88∶1,V/V),检测波长分别为323nm(通道1)、230nm(通道2)。结果显示:芍药苷、阿魏酸分别在21.4~214.0和1.65~16.50μg·mL-1范围内本法有良好的线性关系;平均回收率分别为98.1%(RSD=1.28%)和97.5%(RSD=1.73%)。本法操作简便,快速,重现性好,结果准确,可作为参茸补酒的质量控制方法。 相似文献
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采用高效液相色谱(HPLC)法,用C18色谱柱,甲醇-水-冰乙酸为(55:45:1,V/V/V)流动相,在波长276 nm处测定感冒止咳颗粒中黄芩苷的含量.黄芩苷在0.101~1.01μg范围内与峰面积有良好的线性关系(r=0.9998),平均回收率为100.26%,相对标准偏差为1.52%(n=6).该法操作简便,分析速度快,结果准确,可用于感冒止咳颗粒中黄芩苷含量的测定. 相似文献
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HPLC法同时测定红景天中红景天苷、酪醇和没食子酸 总被引:2,自引:0,他引:2
用高效液相色谱法同时测定大花红景天中红景天苷、酪醇和没食子酸的含量.采用C18 (4.6 mm×200 mm,5 μm)色谱柱,V(甲醇)∶V(0.5%磷酸水溶液)=5∶95为流动相,流速1.0 mL/min,柱温40 ℃,在278 nm下进行检测.大花红景天中红景天苷、酪醇和没食子酸的平均含量分别为3.06%,0.78%和0.18%.平均回收率分别为99.90% (RSD=1.86%)、100.70% (RSD=0.74%)和99.10% (RSD=1.64%).该方法可用于测定红景天中红景天苷、酪醇和没食子酸的含量. 相似文献
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本文利用高效液相色谱法同时测定中药贯叶连翘中绿原酸、芦丁、金丝桃苷和槲皮素四种成分的含量。采用Tiahhe Kromasil C18 100 A(5μm,250mm×4.6 mm)反相色谱柱;流动相为V(乙腈)∶V(水)=20∶80(含0.02%三氟乙酸);紫外检测波长270nm;流速1.0 ml/min;柱温40℃。绿原酸、芦丁、金丝桃苷和槲皮素线性范围分别为3.4~34μg.mL-1(r=0.9993),1.8~18μg.mL-1(r=0.9998),2.3~23μg.mL-1(r=0.9999),3.5~35μg.mL-1(r=0.9991),平均回收率(n=5)分别为98.4%(RSD=1.48%),101.8%(RSD=0.74%),103.7%(RSD=0.77%),103.5%(RSD=1.28%)。方法线性范围宽、相对标准偏差低、精密度高、重现性好,应用于贯叶连翘及制剂样品的测定,结果令人满意。 相似文献
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建立同时测定百合固金颗粒中芍药苷和甘草苷含量的高效液相色谱法。采用Welch Ultimate XB–C18色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈–0.1%磷酸(体积比为14∶86),流速为1.0 m L/min,柱温为30℃,检测波长为230 nm。百合固金颗粒中芍药苷在14.91~149.12 ng,甘草苷在34.75~347.52 ng范围内均有良好线性,线性相关系数分别为0.999 5,0.999 2,平均回收率分别为96.7%,95.9%,测定结果的相对标准偏差小于3%(n=6)。该方法操作简单,专属性强,准确度高,重复性好,可以有效地控制百合固金颗粒的质量。 相似文献
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柱前衍生,高效液相色谱法测定蓝莓果汁饮料中花色苷的含量。在温度为353K条件下,蓝莓果汁饮料与25%盐酸/甲醇溶液(V∶V=1∶1)反应1h,经过0.45μm微孔滤膜过滤后,采用高效液相色谱配二极管阵列检测器检测,以氯化矢车菊素为参照,外标法计算含量。采用Agilent HC-C18柱(250mm×4.6 mm,5μm),流动相A:0.4%三氟乙酸(TFA)水溶液,流动相B:0.4%TFA/乙腈溶液,梯度洗脱,流速1m L·min-1,进样体积20μL,柱温35℃,检测波长为190~800 nm,定量波长520nm。平均加标回收率为94.8%~98.0%,RSD为2.83%,检出限为0.008μg·m L-1。该方法简单、快速、成本低,适用于蓝莓果汁饮料中花色苷含量的测定。 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