鼠李糖脂应用于微乳毛细管电动色谱快速测定化妆品中激素类物质

采用生物表面活性剂鼠李糖脂建立了无需助表面活性剂的微乳体系,并应用于微乳毛细管电动色谱快速分析化妆品中皮质类激素泼尼松、泼尼松龙和氢化可的松。考察了pH值、鼠李糖脂浓度、离子强度、油相种类和浓度、分离温度、分离电压及进样电压和时间的影响,得出微乳体系最佳组成为0.1%(w/w)鼠李糖脂+0.8%(w/w)正庚烷+99.1%(w/w)硼砂缓冲液(80 mmol/L,pH 9.2)。分离温度20℃,分离电压20kV,电动进样10 kV×3 s,泼尼松、氢化可的松和泼尼松龙在9.4 min内可基线分离。重复进样7次,迁移时间和峰面积的RSD分别小于0.2%和5.0%。3种分析物线性范围均为5～100 mg/L;检出限分别为1.0,1.1和1.3 mg/L(S/N=3)。仅需简单萃取即可用于化妆品样品测定,回收率为81.6%～108%;RSD均小于4.8%。     

Desirability-based optimization and its sensitivity analysis for the perindopril and its impurities analysis in a microemulsion LC system

In the current paper the application of multiobjective optimization (MOOP) technique, via Derringer's desirability function, to a microemulsion liquid chromatographic (MELC) method is described. Chromatographic separation of perindopril tert-butylamine and its four impurities was selected as the case study. Central composite design (CCD) with fractional factorial design, ± 0.5 α star design and four replications in central point was applied for a response surface study, in order to examine in depth the effects of the most important factors. As factors that influence the system mostly (i) content of ethyl acetate and (ii) butyl acetate in composite internal phase, (iii) content of sodium dodecyl sulfate (surfactant) and (iv) n-butanol (co-surfactant), as well as (v) pH of the mobile phase were selected. Retention factor of (a) perindoprilat and (b) impurity Y 31 and (c) resolution factor for impurities Y 32 and 33 were chosen for simultaneous optimization. By adjustment of the importance coefficients and weights, according to defined objectives, the optimal mobile phase composition was predicted to be: 0.24% w/v butyl acetate, 0.3% w/v ethyl acetate, 2% w/v SDS, 7.75% w/v n-butanol and pH of the mobile phase 3.7. The sensitivity analysis of desirability function for these optimal conditions was conducted for the first time in LC separations, by applying a sensitivity procedure. The performed sensitivity analysis confirmed that the higher overall desirability does not necessarily mean a better solution. The accuracy of prediction might be affected if the optimal levels of input variables, achieved from several design points, end up with equal settings and different corresponding overall desirability. In our study this was not the issue, which confirmed the adequacy of predicted optimum.     

微乳液高效液相色谱的发展与应用

综述了过去十年中微乳液高效液相色谱法的发展与应用,主要涉及溶质的迁移行为及其影响因素和微乳液高效液相色谱在药物分析中的应用(引用文献33篇)。     

十二烷基硫酸钠微乳色谱体系中pH值对其电渗流行为与微结构的影响

以十二烷基硫酸钠(SDS)/正己烷/正丁醇/硼砂微乳液为毛细管电色谱运行研究体系,以甲醇峰为微乳体系电渗流峰(EOF),考察不同pH值条件下微乳体系电渗流出峰时间(tEOF)和变化趋势.以微乳液滴粒径和ξ电位考察pH值对SDS缓冲溶液微乳体系微结构的影响,用微乳体系的电导值分析pH值条件下微乳液滴与氢氧根离子之间的相互...     

微乳液进样火焰原子吸收光度法测定食品中的微量锰

研究了多种表面活性剂及微乳液对火焰原子吸收光谱法测定锰的增敏作用，并选择增敏作用最强的微乳液作为锰测定的增敏试剂，拟定了测定锰的新方法。     

Rapid dissolution of vitamin E by using sodium N-lauroylsarcosinate ionic surfactant

Vitamin E is widely used in pharmaceutical, food and cosmetic preparations. This paper discusses methods of preparing a vitamin E emulsion by using sodium N-lauroylsarcosinate (SNLS) ionic surfactant. The amount of vitamin E dissolved in water was analyzed by turbidity and UV absorption measurements. The emulsion droplet size was determined by laser light scattering. Microemulsions with small particle size and high resistance to oxidation in air can be obtained by solubilizing vitamin E in SNLS solution. The dissolution is rapid and the surfactant solution has high solubilization power. At 0.7% surfactant concentration, the saturation value is 1 g vitamin E per gram of surfactant. The micellar dissociation concentration (MDC) of the surfactant can be estimated from a vitamin saturation—surfactant concentration curve. Dissolution mechanisms at different surfactant concentrations are interpreted by use of the MDC and CMC (critical micellar concentration) concepts.     

Elastically-induced shift of system-spanning cluster formation in water/oil-microemulsion networks

The influence of ABA-triblock copolymers on the temperature-induced infinite droplet cluster formation in water/oil-microemulsions is studied. The effects of the different blocks of the polymer can be well separated. With the help of an Ehrenfest relation the coupling between the elastically-induced shift of the infinite cluster formation temperature T_c and the plateau modulus of the resulting microemulsion networks is described.     

Influence of pyridine oximate and quaternized pyridinium oximate ions on the hydrolysis of phosphate esters in cationic microemulsions

Kinetic studies have been performed to understand the hydrolytic potencies of oximate (2- and 4-pyridinealdoxime) and its functionalized oximate (4-(hydroxyiminomethyl)-1-alkylpyridinium bromide) ions (alkyl?=?C₁₀H₂₁ (4-C₁₀PyOx^-); alkyl?=?C₁₂H₂₅ (4-C₁₂PyOx^-)) in the cleavage of phosphate esters, diethyl p-nitrophenylphosphate (Paraoxon) and p-nitrophenyl diphenyl phosphate (PNPDPP) in a cationic (O/W) microemulsion system (ME) over a pH range 7.5 to 11.0 at 300?K. The k_obs values for the reaction of paraoxon with oximate and its functionalized oximate were determined in different microemulsion composition and the kinetic rate data shows that k_obs values increases with increasing water content. The specificity of different chain length of alcohols (n-butanol, n-pentanol, n-hexanol and n-octanol) was also investigated in hydrolytic reactions of paraoxon for different microemulsion composition.     

微乳电动色谱法的研究进展

微乳电动色谱(MEEKC)是一种以微乳为背景电解质,以电压为驱动力的分离技术。本文对MEEKC中的各调节参数进行了概述,重点归纳了MEEKC法在正辛醇-水分配系数测定、中药和手性化合物分离方面的应用,以及在操作技术上的新进展,如多路进样技术以及在线联用质谱检测技术等,并通过对相关文献的分析,对一直存有争议的MEEKC与胶束电动色谱(MEKC)的联系与区别进行了讨论,最后提出了MEEKC法未来的发展空间。     

The study on preparing anti-radiation material by reverse microemulsion method

A new way to prepare PMMA contain lead salt was presented. This work firstly prepares the material by microemulsion polymerization. The ability of anti-radiation, transmittance ratio and glass transition temperature （Tg） of the material was characterized. The anti-radiation ability is enhanced with the increasing of lead salt content and the thickness of the material. The transmittance ratio decreased with the content of the lead salt. The glass transition temperature of the material is increased with the lead salt content of the organic glass.