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Capillary Electrophoresis Chiral Separation for Enantiomeric Purity Determination of a Basic Drug in Pharmaceutical Formulations 总被引:1,自引:0,他引:1
Capillary electrophoresis using a running buffer composed of β-cyclodextrin as the chiral selector and ethanolamine mesylate at pH 9.6 is being used to monitor the stereochemical stability of a hydrophobic drug, containing two chiral centers, in two different formulated self-emulsifying drug delivery system (SEDDS) products. The separation takes place in less than 25 min. Strategies for enhancing the method reproducibility and detection sensitivity in the lower potency formulation are presented. The results demonstrating the specificity, assay precision, recovery, linearity and range achieved during the method validation experiments are presented in this paper.Presented at: CE in the Biotechnology and Pharmaceutical Industries: 7th Symposium on the Practical Applications for the Analysis of Proteins, Nucleotides and Small Molecules, Montreal, Canada, August 12–16, 2005. 相似文献
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《Analytical letters》2012,45(14):2608-2620
Abstract A capillary zone electrophoresis (CZE) method has been developed for the determination of the antibiotic sparfloxacin in tablets. The CZE separation was performed using 75 µm×35 cm fused-silica capillary under the following conditions: 25°C; applied voltage, 12 kV; 25 mM H3PO4-NaOH running buffer (pH 8.5). The detection wavelength was 254 nm. Flumequine was used as internal standard (IS). The method was suitably validated with respect to linearity, limit of detection and quantification, accuracy, precision, specificity, and robustness. The calibration was linear from 10 to 60 µg mL?1 and the limit of detection and quantification were 5.38 and 9.46 µg mL?1, respectively. Recoveries ranging from 95.68%–102.4% were obtained in the determination of sparfloxacin that were spiked to placebos. Excipients in the commercial tablets and degraded products from different stress conditions did not interfere in the assay. The method was successfully applied to the determination of sparfloxacin in pharmaceutical tablets. 相似文献
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毛细管电泳接触反应法测定血清中铁传递蛋白的浓度 总被引:3,自引:0,他引:3
建立了一种测定血清中铁传递蛋白的毛细管电泳接触反应方法,利用血清中铁传递蛋白计算化学结合铁的性质,用标准铁饮和铁传递蛋通过对铁准确定量,测定血清铁伟递蛋白的有浓度。 相似文献
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SeparationandDeterminationofBasesbyCapillaryZoneElectrophoresisZHAOTao,LIUQi-ping,CHENGJie-ke(DepartmentofChemistry,WuhanUniv... 相似文献
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毛细管电泳法快速测定淀粉中可乐定 总被引:2,自引:0,他引:2
提出了毛细管电泳快速测定淀粉中可乐定含量的方法。以pH 2.2的磷酸-25 mmol.L-1磷酸二氢钠缓冲溶液为电解质溶液,分离电压20 kV,于214 nm波长处进行紫外检测。在优化的试验条件下,可乐定的质量浓度在0.3~200 mg.L-1范围内与其对应的校正峰面积呈线性关系。检出限(3S/N)为0.1 mg.L-1,测定下限(10S/N)为0.3 mg.L-1。采用该方法对淀粉样品中可乐定含量进行测定,所得加标回收率在97.1%~98.4%之间,相对标准偏差(n=5)小于2.0%。 相似文献
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毛细管电泳进样技术新进展 总被引:2,自引:0,他引:2
评述了毛细管电泳进样技术新成果。对直接在线进样,二维分离体系中毛细管电泳分离的增样,相关毛细管电泳增样,超微量样品及单个分子的进样,近端进样,双向进样和高温下的进样装置的应用状况作了介绍。 相似文献
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报道了一种快速,准确的天麻注射液中天麻素含量的毛细管电泳测定法。方法的线性范围为80-1500μg/mL,RSD=1.90%(n=6)加入回收率为98.9-106.8%。 相似文献
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In this study, we developed an analytical method for the enantioseparation of ofloxacin, using capillary electrophoresis with fluorescence detection. The optimum background electrolyte was obtained to be 60 mM hydroxylpropyl‐β‐cyclodextrin (HP‐β‐CD) in 50 mM phosphate buffer at pH 2.30. Under these conditions, the (+) and (‐) ofloxacin were completely separated, with the detection limit of 10 nM when the sample was prepared in deionized water. The linear ranges of levofloxacin in deionized water and untreated urine were 10?7 to 5 × 10?3 M with R2 = 0.9989 and 5 × 10?6to 5 × 10?3 M with R2 = 0.9943, respectively. We also applied this method to investigate the purity of a commercial drug. The results revealed that the ratio between (+)‐ofloxacin and (‐)‐ofloxacin (levofloxacin) was 99.9:0.1, and there is about 93 mg levofloxacin per tablet (200 mg). The concentration of levofloxacin in patient's urine was founded to be 7.9 × 10?4M, and the ratio between the two optical isomers was 99.3:0.7. 相似文献
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《中国化学会会志》2018,65(4):465-471
Electrophoretic behavior of seven benzophenones as a function of the buffer pH was investigated, and their pKa values were determined by capillary zone electrophoresis. The determination of pKa allows us to rationalize the influence of the buffer pH on the migration behavior of benzophenones. The results reveal that both the presence of intramolecular hydrogen bond and the favorable π‐electronic delocalization decrease the degree of the acid dissociation of the hydroxyl groups of hydroxybenzophenones. However, the introduction of a hydroxyl group at the 4‐position or at the 2′‐position of the aromatic ring of hydroxybenzophenones would decrease greatly their pKa1 values. Thus the presence of this type of hydrogen bonding also plays an important role in the acid dissociation of these hydroxybenzophenones. 相似文献
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A simple, rapid and inexpensive capillary electrophoretic method has been developed and validated for the determination of tadalafil in pharmaceutical preparations. The analysis was carried out using a fused silica capillary (60 cm × 75 m I.D.), phosphate buffer (50 mM, 3.0 pH) as back ground electrolyte (BGE), 15 kV applied voltage with UV detection at 254 nm and at a working temperature of 23 ± 1 °C. Linearity was observed in the concentration range from 200–5000 g/mL, with a correlation coefficient (R2) of 0.9998 and 200 g/mL as the limit of detection. The percentage recovery of tadalafil from pharmaceutical preparations was 99.5. Validation parameters prove the precision of the method and its applicability for the determination of tadalafil in pharmaceutical tablet formulations. The method is fast and is suitable for high throughput analysis of the drug. 相似文献
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牡丹皮中有效成分丹皮酚的毛细管电泳快速检测新方法 总被引:8,自引:0,他引:8
采用毛细管电泳高频电导法对丹皮酚进行了快速分离检测。对电泳介质的种类及浓度、操作电压和进样时间等影响因素进行了优化。最佳条件为:分离介质1.0mmol/LH3BO3-3.0mmol/L三乙胺-10%CH,OH(pH=8.0),分离电压20.0kV,25.0cm位差虹吸进样8.0s。在该条件下。可在4min内实现对丹皮酚的分离检测。线性范围为2.0~105μg/mL,检出限为0.3μg/mL。成功测定了中药牡丹皮中的丹皮酚,回收率达94%~99%。方法简便、快速、灵敏,可用于药物分析。 相似文献
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采用高效毛细管电泳分离并测定了甘草草药和复方甘草合剂中的甘草素和异甘草素的含量。研究了实验参数对分离、检测的影响,得到了优化的实验条件。在50mmol/L硼砂缓冲溶液(pH=9.0)中,甘草素和异甘草素在7min内得到良好的分离。甘草素和异甘草素分别在1.0×10-4~5.0×10-7g/mL、5.0×10-4~1.0×10-6g/mL范围内与电泳峰高呈良好的线性关系,检出限分别为5.0×10-8和2.0×10-7g/mL,已成功地应用于实际样品的测定。 相似文献
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采用毛细管电泳法,以15 mmol·L-1磷酸氢二钠、15 mmol·L-1硼砂和20%乙醇的缓冲溶液作为运行电解质溶液,获得了五味子甲素与五味子中其余成分的有效分离,且峰形较好.测得五味子甲素线性回归方程为y=-0.72+24.9 x,相关系数为0.998;线性范围为0.03~0.37 g·L-1.测得的五味子中五味子甲素质量分数为1.18%,相对标准偏差为2.63%(n=6);平均回收率为99.6%. 相似文献
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《Analytical letters》2012,45(18):2819-2832
The goal of this study was to optimize the parameters for capillary electrophoresis to separate and determine aesculin, aesculetin, umbelliferone, and dihydrocoumarin in plant materials. A simple and rapid capillary zone electrophoresis method is reported for this separation that required less than nine minutes. A bare fused silica capillary was employed using 20 mM borax in 5% methanol at pH 10.1 as the background electrolyte with an applied voltage of 30 kV at 27°C. Good linearity and reproducibility were obtained with high correlation coefficients. The analytes were determined by molecular absorption at 194 and 206 nm. Coumarins were determined in Aesculus hippocastanum L., Cichorium intybus L., Melilotus officinalis L., and Juniperus communis L. “Pendula.” The concentrations of aesculin and aesculetin were 3.07 and 6.31 mg g?1 in Aesculus hippocastanum. In Cichorium intybus, the aesculetin concentration was 2.42 mg g?1. The dihydrocoumarin concentration was 0.54 mg g?1 in Melilotus officinalis, and the concentration of umbelliferone was 0.58 mg g?1 in Juniperus communis “Pendula.” 相似文献