Determination of major aromatic constituents in vanilla using an on‐line supercritical fluid extraction coupled with supercritical fluid chromatography

Abstract

An on-line supercritical fluid extraction coupled with supercritical fluid chromatography method was developed for the determination of four major aromatic constituents in vanilla. The parameters of supercritical fluid extraction were systematically investigated using single factor optimization experiments and response surface methodology by a Box-Behnken design. The modifier ratio, split ratio, and the extraction temperature and pressure were the major parameters which have significant effects on the extraction. While the static extraction time, dynamic extraction time, and recycle time had little influence on the compounds with low polarity. Under the optimized conditions, the relative extraction efficiencies of all the constituents reached 89.0-95.1%. The limits of quantification were in the range of 1.123-4.747 μg. The limits of detection were in the range of 0.3368-1.424 μg. The recoveries of the four analytes were in the range of 76.1-88.9%. The relative standard deviations of intra- and interday precision ranged from 4.2 to 7.6%. Compared with other off-line methods, the present method obtained higher extraction yields for all four aromatic constituents. Finally, this method has been applied to the analysis of vanilla from different sources. On the basis of the results, the on-line supercritical fluid extraction-supercritical fluid chromatography method shows great promise in the analysis of aromatic constituents in natural products.

Recent advances of online coupling of sample preparation techniques with ultra high performance liquid chromatography and supercritical fluid chromatography

“…When the extraction vessel of 5 mL is used, the supercritical extractant should be split in order to prevent exceeding the maximum injection volume of the chromatographic column, which means only part of the extractant is injected into the column. The split of flow can be realized by adjusting the pressures of the two back pressure regulators to increase the pressure difference .…”

“…When the extraction vessel of 5 mL is used, the supercritical extractant should be split in order to prevent exceeding the maximum injection volume of the chromatographic column, which means only part of the extractant is injected into the column. The split of flow can be realized by adjusting the pressures of the two back pressure regulators to increase the pressure difference [73]. for modifier(s), (5) extraction vessel in extractor unit, (6) backpressure regulator (waste), (7) separation column, (8) UV-VIS detector, (9) make-up solvent, (10) make-up solvent pump, (11) backpressure regulator, (12) mass spectrometer, boxed components are temperature controlled, from [72], with the permission of Elsevier.…”

“…5 Phenol and nitrophenols Tap and river waters. [74] 184 Pesticides Water samples [81] 11 Phenolic compounds Water samples [82] 16 Polycyclic aromatic hydrocarbons Water samples [83] 35 Common contaminants Water samples [84] SFE-SFC direct connected 16 Polycyclic aromatic hydrocarbons Soils [72] 4 Aromatic constituents Vanilla [73] Capsaicinoids Placentas of capsicum [75] Phospholipids profiling Dried plasma spot [76] 4 Hydrophilic metabolites and 17 hydrophobic metabolites Dried serum spots [77] 21 Carotenoids Red habanero peppers [78] Carotenoids and apocarotenoids Intact human blood [79] 8 Ketamine and its metabolites Dried urine [80] was established and was applied to the determination of the phospholipids profiling of dried plasma spot [76]. In this method, only 3 μL of plasma was extracted by SFE in 5 min and was analyzed by SFC within 15 min.…”

“…Liang et al. developed an online SFE‐SFC method to determine the major aromatic constituents in vanilla, and the online method showed highest extraction yield compared with other offline methods with the recoveries in the range of 76.1–88.9% . Online SFE‐SFC was also applied to the determination of targeted carotenoids from red Habanero peppers in <17 min, the extraction time was drastically reduced compared with the traditional solid/liquid extraction which required a few hours .…”

Determination of lipid mediators in breast cancer cells using lyophilization‒supercritical fluid extraction online coupled with supercritical fluid chromatography‒quadrupole tandem mass spectrometry

“…Up to now, the online SFE‒SFC‒MS/MS system has been applied to the determination of lipid metabolites , polycyclic aromatic hydrocarbons , and carotenoids . The samples for the online SFE‒SFC analysis were limited in the dried blood spots , soil , or natural products for the system was not appropriate to analyze samples with water . There has been no report for the analysis of cell samples by online SFE‒SFC‒MS/MS.…”