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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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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
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In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献
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Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described. 相似文献
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用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在. 相似文献
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Jona Mirnik Eva Pušavec Kirar Sebastijan Ričko Uroš Grošelj Amalija Golobič Franc Požgan Bogdan Štefane Jurij Svete 《Tetrahedron》2017,73(24):3329-3337
A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu0 as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than CuI in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT). 相似文献
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George E. Magoulas Thomas Garnelis Constantinos M. Athanassopoulos Dionissios Papaioannou George Mattheolabakis Konstantinos Avgoustakis Dimitra Hadjipavlou-Litina 《Tetrahedron》2012,68(35):7041-7049
(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C60, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine. 相似文献