A capillary electrophoresis method for the determination of soluble monosaccharides in Ginkgo biloba leaves.

A method for the simultaneous determination of six monosaccharides by pre-column derivatization with 1-phenyl-3-methyl-5-pyrazolone and capillary electrophoresis was developed in this work. The derivatization (i.e., reaction temperature, capillary electrophoresis duration, and extraction number) and separation (i.e., pH and buffer concentration) conditions for capillary electrophoresis were optimized. Results showed that the limits of detection under optimal conditions were in the range of 0.036-0.35 mg/L with a mean correlation coefficient >0.99. The recoveries were in the range of 87.3-108.49%, and the relative standard deviations of intra- and inter-day variations were in the ranges of 2.2-3.8 and 3.2-5.0%, respectively. The method was successfully applied to the analysis of six free monosaccharides in three types of Ginkgo biloba leaves.

Simultaneous Detection of Anions and Carbohydrates in Cyanobacteria by Two-Dimensional Ion Chromatography.

BACKGROUND: The simultaneous analysis of several anions and carbohydrates by one-dimensional chromatography with a single detector is often complicated by the presence of overlapping peaks. To overcome this problem, analytes are usually analyzed separately making analysis long and tedious. OBJECTIVE: A method combining two-dimensional ion chromatography (2D-IC) and valve switching was developed for the simultaneous determination of anions (F-, Cl-, NO2-, SO42-, NO3-, and PO43-) and carbohydrates (glycerin, glucosyl glycerol, trehalose, mannose, glucose, galactose, fructose, ribose, and sucrose) in cyanobacteria. METHOD: Interfering color compounds were removed by first passing the sample through graphitized carbon solid phase extraction (SPE) cartridges. Samples were applied to an AS11-HC column, which was used to separate the anions followed by quantification using a conductance detector. Carbohydrates eluted from the AS11-HC column were trapped and separated on a MA1 column and simultaneously quantified using electrochemical detection in the second dimension with valve switching. RESULTS: The following parameters were established: LOD, 0.001-0.030 (mg/L); LOQ, 0.001-0.010 (mg/L); linearity (R2), 0.9940; repeatability, 0.39-3.02%; and spiked recovery, 90.1-107%. CONCLUSIONS: The proposed method is adequately linear, accurate, and repeatable. The 2D-IC method provides fast, high-resolution, and completely automated procedure for the simultaneous determination of anions and carbohydrates without co-elution compared to the 1D ion chromatography method. This study provides application perspectives for use in biotechnology and other research fields. HIGHLIGHTS: An accurate and effective 2D-IC method was developed for determining anions and carbohydrates in cyanobacteria. The method includes pre-treating samples with graphitized carbon SPE cartridges.

A novel imidazolium bonding stationary phase derived from N-(3-aminopropyl)-imidazole for hydrophilic interaction liquid chromatography.

In this work, a novel imidazolium bonding method was proposed for the synthesis of hydrophilic interaction liquid chromatography (HILIC) stationary phases. One obtained stationary phase (SilprAprImCl) was derived from direct reaction between N-(3-aminopropyl)-imidazole and 3-chloropropylated silica gel. Other two materials (SilprAprImBF4 and SilprAprImTf2N) were obtained from SilprAprImCl by ion exchange reaction, respectively. Fourier-transform infrared spectroscopy and elemental analysis afforded the proofs of successful imidazolium immobilization and satisfied bonding efficiency. Various polar compounds such as saccharides, nucleosides, and nucleobases were utilized to evaluate the retention behaviours of these materials in HILIC mode. Different effects from mobile composition, column temperature, imidazolium unite and paired anions (Cl-, BF4-, and Tf2N-) in imidazolium were proved and discussed. Separation mechanism and the role of the imidazolium ions were also investigated in mobile phases with different pH. Moreover, chromatographic stability was evaluated by consecutive injections. Finally, the reliability of these stationary phases was demonstrated by the separation of oligosaccharides in real fructooligosaccharides samples.

Synthesis of novel chiral imidazolium stationary phases and their enantioseparation evaluation by high-performance liquid chromatography.

Two novel chiral stationary phases (CSPs) were prepared by bonding chiral imidazoliums on the surface of silica gel. The chiral imidazoles were derivatized from chiral amines, 1-phenylethylamine and 1-(1-naphthyl)ethylamine. The obtained CSPs were characterized by Fourier Transform Infrared (FT-IR) spectroscopy and elemental analysis (EA), demonstrating the bonding densities of CSP 1 and CSP 2 were 0.43 mmol g-1 and 0.40 mmol g-1, respectively. These two CSPs could be used to availably separate 8 pharmaceuticals, 7 mandelic acid/its derivatives, 2 1-phenylethylamine derivatives, 1 1,1'-bi-2-naphthol, and 1 camphorsulfonic acid in high-performance liquid chromatography (HPLC). It is found that CSP 1 could effectively enantioseparate most chiral analytes, especially the acidic components, while CSP 2 could enantiorecognize all chiral analytes, although a number of components did not achieve baseline separation. Additionally, the effects of mobile phase composition, mobile phase pH and salt content, chiral selector structures, and analyte structures on the enantiorecognitions of the two CSPs were investigated. It is found that high acetonitrile content in mobile phases was conducive to enantiorecognition. Mobile phase pH and salt content could alter the retention behaviors of different enantiomers of the same chiral compound, resulting in better enantioresolution. Moreover, both chiral selector structures and substituted groups of analytes played a significant role in the separation of chiral solutes.