Separation of 23 dansylated amino acids by micellar electrokinetic chromatography at low temperature

Summary The baseline separation of 23 dansylated amino acids (including 3 didansylated species) is reported. Lowering of the analysis temperature and fine control of the surfactant concentration were essential in obtaining this result. Calibration graphs with good linearity were obtained.     

胶束荧光法测定维生素B_2含量

维生素B_2(核黄素)为人体内黄酶类辅基的组成部分,参与人体内的生物氧化作用。药典规定其含量测定用分光光度法,文献报道有高效液相色谱法、荧光法等。但因维生素B_2(V_(B2))遇光易分解,尤其在碱性水溶液中,极易变质。其降解产物为感光黄素,二氢核黄素,光化色素等,因此给测定的准确度和灵敏度造成一定的麻烦,为了提     

Micellar effect in hydroformylation of high olefin catalysed by water-soluble rhodium complexes associated with sulfonated diphosphines

High linear alkenes (1-octene and 1-decene) have been hydroformylated using water-soluble rhodium complexes associated with sulfonated diphosphines in the presence of ionic surfactants or methanol. In all cases, the hydroformylation activities were higher than in experiments without additives. The selectivity in aldehydes was higher when we used cetyltrimethylammonium hydrogensulfate (CTAHSO₄) as the surfactant or methanol as the co-solvent.     

Optimized Method for the Determination of Prednisolone, Zn-Bacitracin and Phenylephrine in Local Pharmaceutical Preparations by Micellar Electrokinetic Capillary Chromatography

Summary A new, rapid and simple method is described and applied to resolve and quantify mixtures of prednisolone, Zn-bacitracin and phenylephrine. The determination was accomplished by MEKC. The separation was carried out at 25 °C and 30 kV, using a 5 mM phosphate-5 mM borate buffer (pH=8.2), 40 mM SDS as background electrolyte. Under these conditions, the run time was 6.6 min and the limits of quantification were about 1.0 mg L^–1 for every component. Repeatability and reproducibility studies were achieved showing no significant differences at 95% confidence level. The MEKC method has been applied for quantifying these compounds in different commercials pharmaceuticals products, without separations steps.     

胶束薄层色谱法测定食品及药用胶囊中的合成食用色素

在聚酰胶片上以13%SDBS(十二烷基苯磺酸钠)+7%Triton X-100〔聚乙二醇-对-(1.1,3,3-四甲基)丁基苯基醚〕+(2+3)氨水(1+5+1)为展开剂,用胶束薄层色谱法分离和测定了柠檬黄、亮蓝、苋菜红、胭脂红和赤藓红。测定波长分别为440、632、535、525和528 nm,线性范围分别为0.1～2、0.05～1、0.05～1、0.05～1和0.05～1μg/斑点。方法用于测定软饮料糖果及药用胶囊中的合成色素,获得了满意的结果。此外,还对展开剂的最佳组成进行了单纯形法优化。     

胶束液相色谱／安培电化学检测尿样中的扑热息痛及4－氨基苯酚

用胶束液相色谱／安培检测器检测尿样中的扑热息痛及其主要水解产物４－氨基苯酚。采用１４．５μｍ的碳纤维电极作为工作电极，以高于临界胶束浓度的阴离子表面活性剂十二烷基磺酸钠（ＳＤＳ）作为液相色谱的流动相，尿样直接进样分析，扑热息痛和４－氨基苯酚的检测限分别为０．１３ｎｍｏｌ／Ｌ及０．７３ｎｍｏｌ／Ｌ（Ｓ／Ｎ＝２）。     

高效毛细管电泳的电导检测和紫外光度检测研究

本文自制商效毛细管电泳装置.研究了毛细管区带电泳电导检测和毛细管胶束电动色谱紫外光度检测。在电导检测中,制作铂丝微电导池,并由用电池隔膜制作的导电接口连接电泳毛细管和电导池,高压被有效隔离,实现柱后电导检测,用内径200μm、长70cm(到接口)石英毛细管在10kV电压下分离检测Li~-、Na~-、K~-。在电动色谱中将高效液相色谱仪与高压电源组成电泳装置,用内径100μm,长50cm(到检测器)石英毛细管和SDS胶束溶液在14kV电压下分离检测电中性化合物。     

用毛细管电泳法对某些药物的分离试验

本文采用毛细管电泳法,以50μm内径,45cm长的弹性石英毛细管作为分离管,选用磷酸盐-硼酸盐-十二烷基硫酸钠缓冲溶液体系,在柱254nm紫外检测器,在不同的电泳电压下,对水溶性维生素,磺胺类药物、头孢菌素抗生素,解热镇痛药物有效成份进行了分析,取得较满意的结果。     

Trace analysis of rapamycin in human blood by micellar electrokinetic chromatography

A capillary electrophoretic method with UV detection at 278 nm has been developed for analysis of the immunosuppressant rapamycin (sirolimus) in human blood at low microgram per liter levels. Separation has been achieved in an acidic carrier electrolyte containing sodium dodecylsulfate and 30% (v/v) acetonitrile. For sample clean-up and preconcentration, an off-line solid-phase extraction step using a silica-based reversed-phase material and an on-capillary focussing technique were employed. The latter allows the injection of increased sample volumes without excessive band broadening. Although this new method is less sensitive than existing liquid chromatographic procedures combined with mass spectrometry, it is fully suited to routine analysis of rapamycin in blood from patients treated with this drug. Last but not least the low costs make it an attractive alternative to established methods.     

Study of urinary nucleosides as biological marker in cancer patients analyzed by micellar electrokinetic capillary chromatography

Thirteen normal and modified nucleosides, primarily degradation products of transfer ribonucleic acid (tRNA), were evaluated as potential tumor markers for cancer patients. Their urinary concentrations were determined by means of micellar electrokinetic capillary chromatography (MEKC) in the urine from 54 healthy adults and 70 cancer patients, then quantitatively expressed as a function of creatinine excretion. It was found that urinary nucleosides for cancer patients were on the average significantly higher than those for healthy controls, however, no significant differences were found between male and female or between different ages. Based on 13 urinary nucleoside concentrations, principal component analysis (PCA) could be used to classify 72% of cancer patients from the healthy controls. The present study shows that the precise measurement of urinary nucleosides by MEKC in combining with PCA technique may provide a clinically useful approach for diagnosis of cancer.