Enantiomeric Separation of Epinephrine and Salbutamol by Micellar Electrokinetic Chromatography Using β-Cyclodextrin as Chiral Additive

Enantiomeric separation of epinephrine and salbutamol was investigated by micellar electrokinetic chromatography employing β-cyclodextrin as chiral additive in ammonium chloride-ammonia solution. The analytes were detected by electrochemistry using gold microelectrode at +0.65 V versus SCE reference electrode. The effects of detection potential, concentration of β-cyclodextrin, concentration of sodium dodecyl sulfate, pH value of electrolyte and applied voltage were discussed.

Simultaneous determination of ten nucleosides and bases in Ganoderma by micellar electrokinetic chromatography

Ganoderma(lingzhi)is a famous herbal medicine and edible supplement in oriental countries for a long history.In this study,a simple micellar electrokinetic chromatography(MEKC)method was established for the analysis of nucleosides and bases,the major bioactive components in Ganoderma for the first time.By optimizing the borate concentration,the sodium dodecyl sulfate(SDS)concentration and the pH value of running buffer,10 nucleosides and bases achieved an ideal separation.In real sample analysis,the developed method was successfully used to determine the 10 target analytes in 23 batches of Ganoderma samples from different regions.Results indicated that contents of 10 investigated analytes in each sample showed obvious variation.The principal components analysis(PCA)and hierarchical cluster analysis(HCA)analysis classified the samples into three groups,and the HCA tree visualized the relationships which was mainly contributed by geographical partition.The results indicated geographical origin to be an important factor that affect the accumulation of nucleosides and bases in Ganoderma.In summary,this study provides a simple and practical strategy for quality assessment and cultivation reference of Ganoderma.

Quantitative analysis of two analgesic formulations by micellar electrokinetic chromatography

A micellar electrokinetic chromatographic (MECC) method with sodium cholate as pseudostationary phase was proposed for the separation and quantitation of two analgesic formulations containing acetaminophen, dextro-methorphan hydrobromide, phenylpropanolamine hydrochloride, and chlorpheniramine maleate. The internal standard method was proved to be able to yield satisfactory results even with a modular CE instrument with RSD between 0.6 similar to 2.1%, and recoveries ranging from 98.1 similar to 99.9%.

Study of Tea Digitized Chromatographic Fingerprint Spectra Using Micellar Electrokinetic Chromatography

This paper described the principle of digitized chromatographic fingerprint spectrum and established digitized chromatographic fingerprint spectra of ten brands of Chinese famous tea by the micellar electrokinetic chromatography. This work was done using a 25 mmol·L -1 sodium dodecylsulfate in a 20 mmol·L -1 borate (pH 7 0) solution as running buffer, 20 kV applied potential and detection at 280 nm. The chromatographic fingerprint spectra were digitized by the relative retention value ( α ) and the relative area ( S r), and were analyzed to identify the tea samples. In the absence of the standard samples, the present method was easy setup and inexpensive, and provided the applicable information for the quality assessment of teas.

Effect of organic modifiers on the capacity factor in micellar electrokinetic chromatography

Organic modifiers were effective both to extend the migration time window and to improve the separation of very hydrophobic compounds in MEKC. An iteration method was used to determine the migration time of micelles. The quantitative relationship between the capacity factor k' and the concentration of organic modifiers was derived, which was investigated experimentally. The linear solvation energy relationships (LSER) methodology was applied to MEKC, and good linear relationships between lnk' and solvatochromic parameters of 15 solutes were obtained in the presence of organic modifier in different concentrations, which indicated a new access in MEKC to predict k' from the structural parameters of solutes. The effect of column temperature T on k' was also investigated.

Enantiomeric Separation of Epinephrine and Salbutamol by Micellar Electrokinetic Chromatography Using β-Cyclodextrin as Chiral Additive

Enantiomeric separations of epinephrine and salbutamol, by means of micellar electrokinetic chromatography (MEKC) employing β-cyclodextrin as chiral additive in ammonium chloride-ammonia solution were investigated. In this system, the analytes migrated with the micellar phase towards the anode and were detected by electrochem- istry using gold microelectrode at +0.65 V vs. SCE. The success of the chiral separations is strongly dependent on the concentration of β-CD and SDS, and the optimal concentration is 8 mmol?L-1 and 15 mmol?L-1 respectively. The effects of detection potential, pH value of electrolyte and applied voltage were discussed also. Using the pro- posed method, baseline separation of the enantiomers could be accomplished in 6 min. Further, an attempt was made to elucidate the plausible mechanism of the chiral recognition.

Pseudo Peak Phenomena in Micellar Electrokinetic Capillary Chromatography by Using Ionic Surfactant

The origin of pseudo peak was studied by means of micellar electrokinetic capillary chromatography with cetyltrimethylaminium bromide as the pseudo stationary phase. It has been pointed that two peaks may appear for one component under certain conditions. Experiments showed that the relative areas of the two peaks of analyte depended on the time and the temperature of reaction between analyte and surfactant, and the concentration of surfactant in the sample solution. It means that the interaction between the analyte and the surfactant is a slow process, and a stable substance can be produced from the interaction. It is the substance and the analyte that may lead to the formation of two peaks. The fast interaction mechanism between the solute and the micellar should be queried from the experiment result.

Separation of Aniline Derivatives by Micellar Electrokinetic Capillary Chromatography

A micellar electrokinetic capillary chromatography (MECC) was developed for the determination of aniline and 6 substituted anilines. The seven components were separated within 25 min in the buffer solution of 40 mmol/L sodium borate and 100 mmol/L SDS. It was found that the separation was dependent on operating voltage, pH value, borate and SDS concentrations. The analytical performance was examined in terms of linear response and reproducibility. Wastewater was determined by the established method.

Separation of Biphenyl Nitrile Compounds by Microemulsion Electrokinetic Chromatography with Mixed Surfactants

A mixture of nine biphenyl nitrile compounds with high hydrophobicity and similar structures was successfully separated by microemulsion electrokinetic chromatography (MEEKC) within 30 min. The buffer system contained 100 mmol/L sodium dodecyl sulfate (SDS), 80 mmol/L sodium cholate (SC), 0.81% heptane, 7.5% n-butanol, 10% acetonitrile and 10 mmol/L borate. The addition of SC, organic modifiers, sample preparation and temperature all showed remarkable effect on the separation. Meanwhile, the MEEKC method was briefly compared with micellar electrokinetic chromatography (MEKC) method.

Optimized Separation of Nine Xanthones by Microemulsion Electrokinetic Chromatography

A microemulsion electrokinetic chromatography method has been firstly used for the separation of the therapeutically important xanthones from Securidaca inappendiculata. The separation of the nine xanthones was systematically optimized with respect to pH, composition of microemulsion, addition of cyclodextrins, applied voltage and column temperature. Baseline separation was successfully achieved for the nine xanthones, which was also compared with that by micellar electrokinetic chromatography.

Determination of phenolic whitening agents in cosmetics by micellar electrokinetic capillary chromatography with amperometric detection

A sensitive method for simultaneous determination of six phenolic whitening agents, including arbutin, phenol, resorcinol, hydroquinone, kojic acid, and salicylic acid in cosmetics has been developed using micellar electrokinetic capillary chromatography with amperometric detection （MECC-AD）. Effects of several factors, such as the pH value and concentration of running buffer, potential applied to the working electrode, separation voltage, and injection time were investigated to obtain optimum conditions for separation and detection. With a 75 cm long fused-silica capillary tube, well-defined separation of six phenolic compounds was achieved in 10 mmol/L SDS/40 mmol/L H3BO3-Na2B407 running buffer （pH 9.0）. Good linear relationship was obtained for each analyte over three orders of magnitude with correlation coefficients （r2） between 0.9985 and 0.9994, and the detection limit （S/N = 3） ranged from 0.04 p^g/mL to 0.45 p^g/mL. The proposed method has been successfully applied for the determination of phenolic whitening agents in real cosmetic samples with satisfactory results, providing an alternative monitoring method for cosmetics safety regulation.

Optimization of micellar electrokinetic capillary chromatography method using central composite design for the analysis of components in Yangwei granule

Central composite design(CCD),together with multiple linear regression,was successfully used to optimize the electrophoretic buffer system of micellar electrokinetic capillary chromatography(MEKC) for the determination of albiflorin,paeoniflorin,liquiritin,and glycyrrhizic acid in the traditional Chinese medicine(TCM) prescription,Yangwei granule.Concentrations of sodium deoxycholate(SDC) and borate,and proportions of ammonia,acetonitrile,and methanol were optimized.The total resolutions of peaks between the analytes and their adjacent peaks in real samples were integrated into the evaluation index of separation efficiency.The optimum electrophoretic buffer contained 80 mmol/L SDC,20 mmol/L borate,5%(v/v) methanol,0.5%(v/v) ammonia,and 5%(v/v) acetonitrile.The correlation coefficients(R 2 ) between the peak areas and the corresponding concentrations of analytes were greater than 0.9956.The limits of detection(LODs) (S/N=3) of the analytes were 0.97-4.00μg/ml.The results indicate the superiority of CCD in optimizing the separation conditions of complex samples such as TCM prescriptions.

Chiral Recognition of Binaphthyl Derivatives with L-Undecyl Leucine Surfactants in the Presence of Sodium and Lysine Counterions

This study investigates the effect of counterions on the chiral recognition of 1,1'-Binaphthyl-2,2'-diamine (BNA) and 1,1'-Binaphthyl-2,2'-diyl hydrogenphosphate (BNP) enantiomers when using an amino acid-based surfactant undecanoyl L-leucine (und-Leu) as the chiral pseudostationary phase in capillary electrophoresis. The effects of using two different counterions (sodium and lysine) on the chiral recognition of binaphthyl derivatives were compared at varying pH conditions. The enantiomeric separation of BNA and BNP enantiomers via capillary electrophoresis, using und-Leu as the chiral recognition medium, significantly improved the enantiomeric resolution in capillary electrophoresis at pH 7 when using Lysine counterions as compared to using sodium as the counterion. More specifically, at a surfactant concentration of 45 mM, at pH 7, a significant increase in chiral selectivity was observed when lysine was used as the counterion compared to sodium. The enantiomeric resolution of BNA and BNP increased by 6-fold and 1.1-fold, respectively, in capillary electrophoresis experiments when lysine was utilized as the counterion compared to using sodium. Furthermore, the retention factor of BNA and BNP enantiomers also increased approximately 3.5-fold and 4-fold, respectively, in the presence of lysine counterions as compared to using sodium counterions. When running buffer in capillary electrophoresis was increased to pH 11, the resolution and retention factors were nearly identical when comparing the effects of the sodium and lysine counterions. This signifies the important role of lysine’s positive net charge on chiral recognition. This study provides insight into the potential advantages of using cationic, pH-dependent counterions such as lysine to significantly improve the chiral recognition of binaphthyl derivatives when using chiral anionic surfactants as the pseudostationary phase in capillary electrophoresis.