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.

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.

Enantioselective Determination of R-(-)-and S-(+)-Mexiletine in Microsomal Incubates by Capillary gas Chromatography

A method for the assay of R ( ) and S (+) mexiletine in rat liver microsomal incubates was developed. The method involved extraction of mexiletine from the microsomal incubates, and formation of mexiletine diastereomeric derivatives with a chiral reagent S ( ) N trifluoroacetyl prolyl chloride. Separation and quantitation of the diastereomeric mexiletine derivatives were carried out by a capillary gas chromatographic system with flame ionization detection. The assay was linear from 5 to 500 μg/ml for each enantiomer. The average recoveries of analytical method were 93 31±5 59% and 93 10±5 11% for R ( ) and S (+) mexiletine, respectively. The limits of detection and quantitation for the method were 1 0 μg/ml and 5 0 μg/ml for the R ( ) and S (+) mexiletine isomers, respectively. The reproducibility in the assay was better than 16.5% (RSD). The method has been applied to the metabolism study of R ( ) and S (+) mexiletine in rat liver microsomal incubates.

Novel guanidinium-based ionic liquids as stationary phases for capillary gas chromatography

The present study describes guanidinium-based ionic liquids（GBILs） as stationary phases for capillary gas chromatography （CGC） and to the best of our knowledge,no related reports are available up to now.In this study,a hexaalkylguanidinium ionic liquid（DOTMG-NTf;） was synthesized and coated statically onto capillary columns.Selectivity of the stationary phase was evaluated by separating Grob test mixture,test mixture,alcohols mixture,and fatty acid methyl esters mixture,and thermal stability was investigated as well.The present study demonstrates that GBILs as CGC stationary phases exhibit satisfactory selectivity and thermal stability and have a great potential as new candidates for CGC stationary phases.

Retention behaviors of novel ionic liquid stationary phases and their selectivity for capillary gas chromatography

One chloride-terminated ionic liquid（CTIL） and two hydroxyl-terminated ionic liquids（HTILs） were synthesized and used as stationary phases for capillary gas chromatography（CGC）.Molecular interactions of these stationary phases were evaluated by Abraham solvation parameter model,indicating that the CTIL exhibits remarkably strong H-bond basicity and the HTILs possess both H-bond basicity and acidity.The molecular interactions were further confirmed by separation of a complex mixture consisting of ketones,aldehydes,esters,alcohols and aromatic compounds.It was found that the obtained solvation parameters correlate well with the chromatographic performances of the analytes in terms of elution order and resolution.The well correlated relationship between the solvation parameters and the selectivity of the CTIL and HTILs stationary phases is quite helpful in predicting and understanding the retention behaviors of different types of analytes on these stationary phases.

Selectivity of guanidinium ionic liquid for capillary gas chromatography

A guanidinium ionic liquid,N,N,N＇,N＇-tetrahexyl-N＂,N＂-dimethylguanidinium bis（trifluoromethane）sulfonylimide（THDMGNTf2）, was synthesized and used as stationary phase for capillary gas chromatography.In comparison with imidazolium ionic liquid stationary phase,the present new stationary phase exhibits quite different selectivity and behaves more like a low polar stationary phase.The guanidinium ionic liquid of THDMG-NTf2 exhibited better separation of Grab test mixture than imidazolium ionic liquid of 1-octyl-3-butylimidazolium bis（trifluoromethane）sulfonylimide（OBIM-NTf2）.Solvation parameter model was also used to evaluate the selectivity of THDMG-NTf2.Additionally,essential oil of Magnolia biondii Pamp was analyzed to further evaluate the selectivity of THDMG-NTf2 for a sample of complicated components.Satisfactory separation of the essential oil was achieved on a THDMG-NTf2 column（10 m） while using a commercial column（30 m） as reference.The present study shows that the guanidinium ionic liquid possesses novel chromatographic selectivity and has great potential for wide applications.

Determination Enantiomer Excess(e.e.%)of Chiral Sharpless Epoxides with β-Cyclodextrin Derivatives as Chiral Stationary Phases of Capillary Gas Chromatography

Using four β-cyclodextrin derivatives, 2,6-di-O-benzyl-3-O-heptanonyl-β-CD, 2,6-di- O-benzyl-3-O-octanonyl-β-CD, 2,3-di-O-benzyl-6-O-heptanonyl-β-CD, and 2,3-di-O-benzyl -6-O- octanonyl-β-CD, as chiral stationary phases of capillary gas chromatography （CGC）, the enantiomers of Sharpless epoxides were well separated. The enantiomer excess values （e.e.%） of some chiral Sharpless epoxides were also determined successfully using these CDs.

SIMULTANEOUS DETERMINATION OF EPHEDRINE AND ITS ANALOGUES IN URINE BY CAPILLARY GAS CHROMATOGRAPHY

A method is developed for the simultaneous determination of ephedrine,pseudoephedrine, norephedrine, norpseudoephedrine and methylephedrine in urine on a capillary column using nitrogen-phosphorus detector.Diphenylamine is used as the internal standard.Calibration graphs are linear down to 1.30ug/ml urine.

A NOVEL DERIVATIVE OF β-CYCLODEXTRIN AS CHIRAL SIATIONARY PHASE IN CAPILLARY GAS CHROMATOGRAPHY

A novel β-cyclodextrin derivative, 2, 6-di-O-butyl-3-O-acetyl-β-cyclodex- trin, was prepared and used as chiral stationary phase for capillary gas chromato- graphic resolution of enantiomers, lhe glass capillary columns with the derivative having low melting point and high thermal stability could produce more than 3000 plates per column meter and have proven to be good chlral columns to separate the enantiomers of some amino acids, derivatives of epoxy ethane and alkyl halide, etc.

ANALYSIS OF VOLATILE CONSTITUENTS OF CHINESE MEDICINAL HERBS BY FLASH DISTILLATION/CAPILLARY GAS CHROMATOGRAPHY/MASS SPECTROMETRY

In present work,the volatile constituents of Curcuma longa L.,A.lancea (Thunb.) DC.,Foeniculum vulgare Mill,and Cinnamomun cassia Presl.have been analyzed by flash distillation/capillary gas chro-matography/mass spectrometry.The results are consistent with those obtained by conventional steam distillation extraction method.The optimum condition of flash distillation has been studied.The experimental results showed that this new technique proved to be a simple,rapid and efficient tool for microanalysis of volatile constituents of Chinese medicinal herbs.

Polysiloxane with Pendant [60]Fulleropyrrolidines as Stationary Phase for Capillary Gas Chromatography

Polysiloxane with pendant [60] fulleropyrrolidines was synthesized and used as the stationary phase for capillary gas chromatography for the first time. A preliminary investigation of its property shows that it has an excellent thermostability and a wide range of allowable operating temperature from 80 degrees C to 360 degrees C.

Separation Properties of a New Polysiloxane-Anchored β-Cyclodextrin Derivative as Gas Chromatography Stationary Phase

A new capillary gas chromatography stationary phase, monokis (2,6 di O benzyl 3 O propyl (3’)) hexakis(2,6 di O benzyl 3 O methyl) β CD bonded polysiloxane, was synthesized. It exhibited separation abilities to disubstituted benzene isomers and some chiral solutes. It was also found that the polarity of CD derivatives can be lowered both by chemically bonding it to polysiloxane and by diluting it in polysiloxane. The separation abilities of the polysiloxane anchored CDs (SP CD) are higher than that of the unbonded CDs (S CD) and the diluted S CD at lower column temperature. Hydrosilylation reaction is one of the best methods to lower the operating temperature of CDs.

Cross-Linked Crown Ether-SE-54 as Stationary Phase for Open-Tubular Column Gas Chromatography

The cross-linking of crown ether-SE-54 in fused-silica capillary columns were initiated by dicumyl peroxide(DCUP),azo-bis-isobutyronitrile (AIBN)and ozone(O_3).Parameters of evaluation such as polarity,selectivity, phase transition temperature and thermal stability were studied and compared with those of poly(crown ether)stationary phase.

Microwave Extraction Followed by Solid-phase Extraction for the Determination of Phthalate Esters in Fish Samples by Gas Chromatography

A new analytical procedure based on solid-phase extraction method coupled to GC-FID has been developed and validated for the determination of five phthalate esters （PAEs） （dimethyl-（DMP）, diethyl-（DEP）, di-n-butyl-（DBP）, di-2-ethylhexyl- （DEHP）, di-n-octyl-（DOP）） in fish samples. There was a good linear relationship in the range of 0.05-10μg with the detection limits of 0.09-0.16ng .The recoveries obtained for PAEs ranged from 88.6% to 96.4%with RSD of 4.2%-10.2%.The applicability of the developed method was demonstrated for real fish samples.

The Enantiomer Separations of Allethrone and Propargyllone Using Two Long Chain Acylated b-Cyclodextrin Derivatives as CGC Capillary Stationary Phases

Using two b-cyclodextrin derivatives (CDs) with long chain of acyl groups as chiral stationary phases (CSPs) of capillary gas chromatography (CGC), the enantiomers of racemic allethrone and propargyllone were well resolved after derived with acetyl chloride. The enantiomer excess values (e.e.%) of 1S-allethrone and 1S-propargyllone were also determined successfully using these CDs.

Capillary Column Coated with Heptakis(2,3, 6-tri-O-octyl)-β-cyclodextrin Using Sol-gel Technology

Heptakis(2, 3, 6-tri-O-octyl)-β-cyclodextrin was coated onto the fused silica capillary by sol-gel technology. Column efficiency and column selectivity were studied. The results indicated that high ability of separation was acquired . Positional isomers of aromatic compounds were well separated.

GC-MS Analysis of Essential Oil Constituents from Buds of Tussilago farfara L.

Aim To analyse the constituents of the essential oils extracted from the buds of Tussilago farfara L. in the GAP Bases of Traditional Chinese Medical Materials and provide scientific basis for quality control. Methods The essential oils were extracted by water-steam distillation and separated by GC capillary column chromatography. The components were quantitatively determined by normalization, and identified by GC-MS. Results GC-MS exhibited 259 peaks and 65 compounds were identified, accounting for 84.62% of the total essential oil. Conclusion In the total essential oil contained in the buds of Tussilago farfara L., copaene （2.36%）, （ ＋ ） -Epi-bicyclosesquiphellandrene （ 3.91% ）, γ- elemene （2.18%）, fl-bisabolene （ 13.93% ）, spathulenol （ 3.44% ） as the sesquiterpenes and its derivatives, and 1-undecene （4.83%）, （ E）-cycloundecene （8.49%）, bicycle [ 10. 1.0] tridec-l-ene （ 1. 45% ）, 1-tridecene （3.44%）, （Z）-7,11-dimethyl-3-methylene-1,6,10-dodecatriene （2.66%）, 1- pentadecene （4.57%）, [ 1R-（ 1R^＊, 4Z, 9S^＊ ） ]-4,11,11-trimethyl-8-methylene-bicyclo [ 7.2.0] undec-4-ene （ 1.03% ）, 6,6-dimethyl-2-methylene-7-（ 3-oxobutylidene ）-oxepan-3-ylmethyl acetic acid ester （2.02%）, 1, E-11, Z-13-heptadecatriene （ 3.72% ）, （ Z, Z, Z） -9,12,15-octadecatrien-l-ol （ 1.85% ）, 3,7,11-trimethyl-dodeca-2,4,6,10-tetraenal （ 1.31% ）, n-hexadecanoic acid （ 3.12% ） , （Z, Z） -9,12-octadecadienoic acid （2.26%）, （ Z, Z, Z） -9,12,15-octadecatrienoic acid methyl ester （ 1.12% ） , heneicosane （ 1.82% ）, and pentacosane （ 1.03% ） are the main components.

GC-MS Analysis of Essential Oil Constituents from Rhizome and Root of Notopterygium forbesii

Aim To analyse the chemical constituents of the essential oil extracted from the rhizome and root of Notopterygium forbesii Boiss. and provide scientific basis for quality control. Methods The total essential oil was extracted by water-steam distillation and separated by capillary gas chromatography (GC). The components were determined by normalization method, and identified by GC-MS. Results GC-MS exhibited 217 peaks and 100 compounds were identified, accounting for 78.3% of the total essential oil. Conclu...