Homochiral metal–organic frameworks (MOFs) have gained much attention because of their chiral properties and disposition for chiral separation. However, the fabrication of high‐quality homochiral MOF membranes remains challenging because of the difficulty in controlling growth of MOF membranes with chiral functionalities. A homochiral zeolitic imidazolate framework‐8 (ZIF‐8) membrane is reported for efficient chiral separation. The membrane is synthesized by incorporating a natural amino acid, l‐histidine (l‐His), into the framework of ZIF‐8. The homochiral l‐His‐ZIF‐8 membrane exhibits a good selectivity for the R‐enantiomer of 1‐phenylethanol over the S‐enantiomer, showing a high enantiomeric excess value up to 76 %.
Comprehensive two-dimensional gas chromatography hyphenated with accurate mass time-of-flight mass spectrometry (GC × GC-accTOFMS) was applied for improved analytical accuracy of saffron analysis, by using retention indices in the two-dimensional separation. This constitutes 3 dimensions of identification. In addition to accTOFMS specificity, and first dimension retention indices ((1)I), a simple method involving direct multiple injections with stepwise isothermal temperature programming is described for construction of isovolatility curves for reference alkane series in GC × GC. This gives access to calculated second dimension retention indices ((2)I). Reliability of the calculated (2)I was evaluated by using a Grob test mixture, and saturated alkanes, revealing good correlation between previously reported I values from the literature, with R(2) correlation being 0.9997. This essentially recognizes the retention property of peaks in the GC × GC 2D space as being reducible to a retention index in each dimension, which should be a valuable tool supporting identification. The benefit of (2)I data, in supplementing (1)I and MS library matching, was clearly demonstrated by the progressive reduction of the number of possible compound matches for peaks observed in saffron. 114 analytes were assessed according to (1)I and (2)I values within ±20 index unit of reference values, and by MS spectrum matching above a match statistic of 750 (including mass accuracy of the molecular ion <20 ppm) and their possible identities derived. The described method provides a new avenue to utilize the full capability of the two-dimensional separation (GC × GC), in combination with MS library matching in complex sample analysis, to provide improved component identification.
Recent advances in multidimensional gas chromatography (MDGC) comprise methods such as multiple heart-cut (H/C) analysis and comprehensive two-dimensional gas chromatography (GC × GC); however, clear approaches to evaluate the MDGC results, choice of the most appropriate method, and optimized separation remain of concern. In order to track the capability of these analytical techniques and select an effective experimental approach, a fundamental approach was developed utilizing a time summation model incorporating temperature-dependent linear solvation energy relationship (LSER). The approach allows prediction of optimized analyte distribution in the 2D space for various MDGC approaches employing different experimental variables such as column lengths, temperature programs, and stationary phase combinations in order to evaluate separation performance (apparent (1)D, (2)D, total number of separated peaks, and orthogonality) for simulated MDGC results. The methodology applied LSER to generate results for nonpolar-polar and polar-nonpolar 2D column configurations for separation of 678 compounds in an oxidized kerosene-based jet fuel sample. Three-dimensional plots were generated in order to illustrate the dependency of separation performance on (2)D column length and number of injections for different stationary phase combinations. With a given limit of analysis time, a MDGC approach to obtain an optimized total separated peak number for a particular column set was proposed depending on (1)D and (2)D analyte peak distribution. This study introduces fundamental concepts and establishes approaches to design effective GC × GC or multiple H/C systems for different column combinations, to provide the best overall separation outcomes with the highest separated peak number and/or orthogonality.
Flavonoids represent one of the more abundant classes of phytochemicals. They are renowned for their health benefits against age-related ailments and diseases. Several chromatography techniques have underpinned many chemical analysis methods, developed for superior flavonoid separation and identification. Among these, GC is one of the most powerful tools in separation science, providing precise measurement of a wide range of flavonoids. Combined with various detectors - most commonly MS-GC offers a sensitive and accurate tool for quantitative and qualitative flavonoids analysis. This review features developments in the application of GC and MS for flavonoids determination during past decades, progressing to recent developments and considering future trends. The review will highlight the state-of-the-art of GC, with opportunities for multidimensional GC analysis also briefly discussed.
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