共查询到18条相似文献,搜索用时 62 毫秒
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建立了加压毛细管电色谱法测定抗真菌药米卡芬净。采用EP-100-20/45-3-C18-BP反相毛细管色谱柱,以乙腈∶2.5 mmol/L磷酸盐缓冲液(p H 6.5)(35∶65)为流动相,检测波长270 nm,分离电压15 k V。米卡芬净在62.5~800μg/ml浓度范围内线性关系良好,平均回收率为99.6%,RSD为1.47%。 相似文献
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介绍了毛细管电色谱的研究进展 ,以各种手性选择剂的发展为线索介绍了毛细管电色谱手性分离的方法及应用 ,探讨了各种实验条件对分析结果的影响 相似文献
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目的 建立抗真菌药物-阿尼芬净关键中间体棘白菌素B(Echinocandin B,ECB)加压毛细管电色谱分析(pCEC)方法.方法 采用流动相为乙腈-4.35mmol/L的磷酸盐缓冲盐(pH 5.5)(52∶48,V/V),等度洗脱,流速为0.08mL/min,紫外检测波长212nm,分离电压-15kV.结果 各组分在0.015~3.84mg/mL范围内线性良好;检出限和定量限分别为15和30μg/mL;日间和日内精密度均小于5%;加样回收率均高于98%.结论 该方法简单方便,重现性好,准确可靠,回收率较高,为阿尼芬净中间体ECB的分析和质量控制提供了新的方法. 相似文献
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毛细管电色谱在分离手性化合物中的应用 总被引:3,自引:0,他引:3
毛细管电色谱(CEC)将高效毛细管电泳(HPCE)和高效液相色谱(HPLC)两者的优势有机结合起来,是一种新型的微分离技术.在此系统介绍了CEC在分离分析手性对映体上的主要分析方式,并对影响手性分离的主要因素作了介绍. 相似文献
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目的:毛细管电色谱在药物分析中的应用研究。方法:结合国内外有关毛细管电色谱的文献资料,综述毛细管电色谱的研究进展、毛细管电色谱整体柱制备新进展及其在药物分析中的应用。结果:毛细管点色谱在分析领域已得到广泛良好的应用。结论:毛细管电色谱拥有广阔的应用前景。 相似文献
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磺胺类药物的毛细管高效液相色谱与电色谱研究 总被引:4,自引:0,他引:4
目的 研究毛细管高效液相色谱(μ-HPLC)和毛细管电色谱(CEC)分离磺胺类药物,建立药物微分离分析方法。方法 用ODS柱为固定相,甲醇和2 mmol·L-1磷酸缓冲液(pH 3.0~7.0)为流动相,电压为0~-15 kV,流速为10 μL·min-1,紫外检测波长254 nm。结果μ-HPLC在甲醇-2 mmol·L-1磷酸缓冲液(30∶70),pH 3.0时5种磺胺类药物实现基线分离;CEC在电压为-5 kV,甲醇-2 mmol·L-1磷酸缓冲液(30∶70),pH 5.0时5种磺胺类药物实现基线分离。结论电渗流随甲醇含量、缓冲液浓度增加而下降,随pH值、电压的增加而增加;溶质的保留值(k)随甲醇含量、缓冲液浓度、电压的增加而下降,随电压增加下降明显的是TMP,随pH值变化较复杂。在相同条件下对5种磺胺类药物的分离,μ-HPLC需67 min,CEC只需25 min,后者更适合于磺胺类药物的快速分离分析。 相似文献
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目的:建立以阳离子表面活性剂碘化四丁基铵为电渗流改性剂,以盐酸去甲万古霉素为手性选择剂的毛细管电泳法分离西替利嗪对映体。方法:考察了盐酸去甲万古霉素浓度、Tris 浓度和缓冲液 pH 对分离的影响,对分离条件进行了优化。结果:在含0.04 g·L~(-1)碘化四丁基铵和1.0 mmol·L~(-1)盐酸去甲万古霉素的25 mmol·L~(-1)Tris 磷酸缓冲液(pH 4.5)的运行电解质体系中,西替利嗪对映体在分离电压为20 kV 的条件下得到良好分离,西替利嗪对映体分离度达1.8。结论:本法可用于西替利嗪对映体的分离。 相似文献
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Danxia Chen Jiajing Wang Yunyun Jiang Tingting Zhou Guorong Fan Yutian Wu 《Journal of pharmaceutical and biomedical analysis》2009,50(5):695-702
The pressurized capillary electrochromatography (pCEC) was utilized for the separation and determination of coumarins in Fructus cnidii extracts from 12 different regions. After a thorough study of analytical parameters such as acetonitrile content of the mobile phase, the concentration and pH of the buffer, and the applied voltage, a methodology was proposed to separate and determine six coumarins of F. cnidii extracts in less than 15 min. The experiments were performed in an in-house packed column with a monolithic outlet frit under the optimal conditions: pH 4.0 ammonium acetate buffer at 10 mM containing 50% acetonitrile at −6 kV applied voltage. The calibration curves were linear in the range of 10.0–100.0 μg/mL for bergapten, 20.0–200.0 μg/mL for imperatorin, 5.0–400.0 μg/mL for osthole, 10.0–100.0 μg/mL for 2′-acetylangelicin, 10.0–200.0 μg/mL for oroselone, and 10.0–200.0 μg/mL for O-acetylcolumbianetin. The correlation coefficients were between 0.9967 and 0.9995. With this pCEC system, fingerprints of F. cnidii extracts were preliminarily established to distinguish three types of coumarins by characteristic peaks, and the quality of various sources of raw materials was evaluated by determining the contents of six coumarins. 相似文献
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目的:建立毛细管电色谱(CEC)分离检测生物样品中硝基精氨酸异构体的方法。方法:采用CEC手性配体交换模式检测血浆样品中D-硝基精氨酸(D—NNA)和L-硝基精氨酸(L—NNA),流动相为50mmol/L醋酸缓冲液[pH5.0,含2mmol/Laspartame,1mmol/L Cu^2+和5%(v/v)甲醇];流速为0.02mL/min;操作压为1000psi;检测波长为UV280nm。结果:L—NNA和D—NNA在0.025~0.75mmol/L的浓度范围内峰面积/浓度的相关系数均可达0.99以上,日内变异系数均小于3.0%,日间变异系数分别为3.1%和3.4%。结论:本研究方法具有快速、高分辨、检测样品量和流动相用量少等优点。 相似文献
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目的:采用毛细管区带电泳法对盐酸美沙酮对映体进行了拆分。方法:比较了3种衍生化β-环糊精为手性添加剂的分离效果,对缓冲液的pH及浓度、手性添加剂的浓度、柱温、分离电压等方面进行了考察及优化。结果:确定采用75μm×75 cm未凃渍石英玻璃管柱,运行缓冲液为含50 mmol.L-1的Tris和10 mmol.L-1的HP-β-环糊精的水溶液(以磷酸调节pH至2.0),分离电压为25 kV,柱温25℃,检测波长为205 nm,结论:该方法简便、快速,在15 min内分离度可达到1.9。 相似文献
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Lü H Wang J Wang X Lin X Wu X Xie Z 《Journal of pharmaceutical and biomedical analysis》2007,43(1):352-357
A pressurized capillary electrochromatography (pCEC) with monolithic column has been developed for the rapid separation and determination of five structurally related anthraquinones in Rhubarb. The possibility of rapid separation resulted from the unique pore structure with high permeability and favorable mass transfer characteristics of the monolithic stationary phase. The effect factors such as organic modifier, acidity and concentration of running buffer, separation voltage were investigated to acquire the optimum condition. In the 220 nm wavelengths, the five anthraquinones could be baseline-separated rapidly within 5 min with the separation voltage of -20 kV in 10 mmol/L phosphate buffer (pH 6.2) containing 65% acetonitrile. The calibration graphs of rhein, aloe-emodin, emodin chrysophanol and physcion were linear by plotting the peak area against the analytes concentration over the range of 0.2-65, 0.1-30, 0.1-55, 0.5-30 and 0.5-55 microg/mL, respectively. The detection limits of five anthraquinones were ranged from 0.06 to 0.2 microg/mL and the recoveries of Rhubarb samples were about 81.3-86.4% (R.S.D.< or = 5.2%). This proposed method was successfully applied to determination of the five analytes in Rhubarb with satisfactory results. 相似文献
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Chankvetadze B Kartozia I Yamamoto C Okamoto Y Blaschke G 《Journal of pharmaceutical and biomedical analysis》2003,30(6):1897-1906
In the last few years, it has been shown that capillary electrochromatography (CEC) is a promising technique for enantioseparations. However, to date almost no studies are published on a critical comparison of CEC and its pressure-driven counterpart, capillary liquid chromatography (CLC) for real samples. In this study, the goal was to compare CLC and CEC for the determination of the enantiomeric purity of the contraceptive drug levonorgestrel and its pharmaceutical formulation. The study prevailed that not all potential advantages of CEC over CLC can easily be transformed in a real gain of detection limit of the enantiomeric impurity. However, certain advantages of CEC over CLC have been unambiguously shown. 相似文献