The main components in roseous liquid were analyzed qualitatively by GC-MS combination method.The results indicated that 6 organic compounds which had never been reported till now were separated from the extract of hawthorn kernel oil.
A new method has been developed for preparing monolithic materials by polymerisation of the oil-in-water (O/W) emulsions with nonion-surfactant (Pluronic F68). Morphology of monolithic materials is studied by scanning electron microscopy. The properties of the column are investigated, and the column exhibits the ability of low backpressure and fast analysis. Using this monolithic column, on-line sample clean-up and screening of m-nisoldipine in human plasma samples have been investigated. Chromatography is performed by reversed-phase high-performance liquid chromatography (RP-HPLC) on a C(18) column with UV detection at 237 nm. The linear range of m-nisoldipine in human plasma is 2-200 ng/mL (r = 0.9992, n = 7). And the limit of detection is 1.5 ng/mL. The 12-h pharmacokinetic profile of m-nisoldipine in mice after oral administration has been investigated. The results indicate that the method could be used for monitoring of m-nisoldipine and enabled simple and rapid assay of the drugs in human plasma.
A method based on cloud point extraction was developed to determine benzoic acid in milk using high-performance liquid chromatography detection.The non-ionic surfactant Tween-20 was chosen as extraction solvent,the extraction parameters affecting extraction efficiency,such as concentrations of Tween-20 and(NH4)2SO4,equilibration temperature,equilibration time and pH were evaluated and optimized.The optimum CPE conditions were:3%(V/V)Tween-20,300g/L(NH4)2SO4,pH4,equilibration temperature 90℃ for 10min;chromatographic conditions were:mobile phase of ammonium acetate buffer-methanol 90:10(V/V),flow rate 1mL/min,the detection wave length 230nm.Under the above optimized conditions,the linearity of the calibration curve for benzoic acid was in the range of 0.2~2.0μg/mL,the limits of detection was 0.025μg/mL,the correlation coefficient was 0.9998.The recovery for the standard addition of the benzoic acid in the milk ranged from 98.90% to 100.16%,the relative standard deviations was in the range of 1.2%~2.5%.
An aryl-bonded silica column for high performance liquid chromatography was prepared by coupling silica with γ-glycidoxypropyltrimethoxysilane and modifying the stationary phase with ethylenediamine to form amino-group,and then immobilizing p-toluenesulfonic acid onto the monolithic silica columns. The as-prepared aryl-bonded monolithic silica column was characterized with FTIR. Its’ chromatographic properties were evaluated by lysozyme (Lys),human immunoglobulin (IgG) and bovine serum albumin (BSA). Column back-pressure,separation efficiency,loading capacity and the range of pH were also evaluated for fast separation. The results showed that the stationary phase had fine chromatographic properties and good stability with the pH between 2 and 8. The column back-pressure was weakly influenced by flow rate. Therefore,the aryl-bonded monolithic silica column could be used for the fast separation.
A method of micellar electrokinetic chromatography capillary (MECC) has been established for separating polymyxins E1 and E2 in polymyxin E sulfate and determining the contents of E1 and E2. Several factors including the running voltage, the type of surfactant, concentrations of Brij-35 (polyoxyethylene glycol dodecyl ether), NaCl solution and acetonitrile, pH of phosphate were investigated. Under the optimum conditions (10 kV running voltage, phosphate buffer solution (0.01 mol/L, pH 4.1) containing 30 mmol/L Brij-35, 5% (v/v) acetonitrile, 0.167 mol/L NaCl), E1 and E2 were separated with the resolution of 1.94. The contents of E1 and E2 in polymyxin E sulfate were 67% and 32%, respectively. As an example, the relative standard deviations of the intra-assay and inter-assay of polymyxin E1 on the plate number and peak area were less than 5%. The method is simple, rapid, accurate, and reproducible.