Separation and identification of compounds in Adinandra nitida by comprehensive two-dimensional liquid chromatography coupled to atmospheric pressure chemical ionization source ion trap tandem mass spectrometry

Abstract

A comprehensive two-dimensional liquid chromatographic (2D-LC) separation system based on the combination of a CN column and a Merck Chromolith Flash reversed-phase column was developed for the separation of components in Adinandra nitida, one type of traditional Chinese medicine (TCM). The two dimensions were connected by a ten-port, dual-position valve controlled automatically by software written in-house. The effluents were detected by both ultraviolet and atmospheric pressure chemical ionization source ion trap tandem mass spectrometry (MS). The calculated peak capacity of the 2D-LC-MS/MS system was above 1240. More than 57 components were resolved in the methanol extract from Adinandra nitida leaves, and five of these were identified based on their relative retention times, molecular weights and MS/MS spectra.

Comprehensive hydrophilic interaction and ion-pair reversed-phase liquid chromatography for analysis of di- to deca-oligonucleotides

“…As on average each peak was sampled for about 2.7 times for re-analysis in the second dimension, n c dim1 is 20 (=55/2.7). This corresponds to the ratio of number of samplings to the number of samplings per solute [45]. As n c dim2 is estimated at 25 making use of the equation for gradient analysis [43], the overall LC × LC peak capacity is ca.…”

Integration of normal phase liquid chromatography with supercritical fluid chromatography for analysis of fruiting bodies of Ganoderma lucidum

“…Therefore, the peak capacity was improved to 350 within 2 h analysis, which was obviously increased compared to one-dimensional separation. Furthermore, compared to other 2-D-HPLC for TCM analysis [28][29][30], the operation time of such platform was rather short, enabling the high-throughput analysis of TCMs.…”

“…Thus, due to the inherence advantages of superior selectivity, high throughput and high speed, SFC was chosen as the second dimension. Also, due to the high permeability and excellent mass-transfer properties of the skeleton [30], a monolithic silica C 18 column was chosen to replace the packed Hypersil-C 18 column in 2-D-NPLC-SFC to fasten the analysis speed. Furthermore, since the usually used mobile phase in NPLC, hexane and isopropanol could be dissolved in supercritical CO 2 , the compatibility of mobile phases is better than 2-D-NPLC-RPLC.…”

“…Ganoderma lucidum is one of the most famous medicinal funguses that have been widely used for thousands of years, which is composed of triterpenoids, polysaccharides, proteins, and other active small molecules [27]. Due to the complexity of TCMs, multi-dimensional separation techniques are required to improve the peak capacity [28][29][30].…”

Application of fractionized sampling and stacking for construction of an interface for online heart-cutting two-dimensional liquid chromatography

“…Development of this powerful separation technique is mostly owed to the emergence of sophisticated interfaces, which efficiently transfer the first dimension ( 1 D) eluate to the second dimension ( 2 D). Various interfaces, such as switching valves coupled with empty storage loops [6][7][8][9][10] or solid-phase extraction (SPE) columns [11][12][13], stop-flow interface [14,15] and interfaces with parallel second dimension columns [16,17] have been successfully developed for 2D LC. More simple, efficient and sophisticated interface apparatus with independent flow programs and valve switching events are needed to develop effective online 2D LC analysis methods.…”