Optimization of High-Performance Liquid Chromatographic Parameters for the Determination of Capsaicinoid Compounds Using the Simplex Method

Abstract

A high-performance liquid chromatographic method was developed for the analysis of capsaicinoid compounds, the pungent principles of capsicum fruits. A sequential simplex method was applied to optimize the chromatographic response function used to assess the quality of separation by varying the chromatographic parameters. The separation was achieved in 11 min using a C-8 column of 15-cm length and 4.6 mm diameter using a UV detector. A flow rate of 1.15 ml min -1 at a column temperature of 43.5˚C using 63.7% methanol in water gave the most efficient separation. The method was found to be suitable for the determination of the major capsaicinoid compounds in the capsicum samples.

Ultrasound-assisted extraction of capsaicinoids from peppers

“…Many different techniques have been employed for the extraction of capsaicinoids from pepper, such as maceration [11], magnetic stirring [12], enzymatic extraction [13], ultrasound-assisted extraction [14], Soxhlet [15], extraction by supercritical fluids [16], extraction by pressurized liquids [17] and microwave-assisted extraction [18,19]. The conventional extraction methods, like Soxhlet extraction, which have been employed for decades, need long extraction times and require relatively large quantities of solvent [20].…”

“…Although studies have been published on the employment of UAE for the recovery of capsaicinoids from peppers [14], these not have evaluated the influence of the extraction variables nor has a systematic study for the optimisation of the method been carried out; therefore no specific protocol for the UAE of capsaicinoids in peppers has been produced. Thus, the object of the work reported here is to perform the optimisation of the various extraction parameters, particularly the appropriate solvent, temperature, extraction time, quantity of sample, etc.…”

“…Methanol [11,14], ethanol [13,17], and acetonitrile [12,31] are solvents that are normally employed for the extraction of capsaicinoids in various extraction techniques, such as Soxhlet extraction, maceration, and extraction by magnetic stirring. Water is not a good solvent for extracting capsaicinoids, but it has been observed that sometimes the addition of small percentages of water to the extraction solvent helps to increase the effectiveness of extraction of the analytes of interest from the sample [26].…”

Determination of capsaicinoids in peppers by microwave-assisted extraction–high-performance liquid chromatography with fluorescence detection

“…Many techniques for the extraction of capsaicinoids from peppers have been studied, such as maceration [9], magnetic stirring [10], Soxhlet [11,12], ultrasound-assisted extraction [13], extraction by means of supercritical fluids [14], extraction by pressurized liquids [15] and enzymatic extraction [16]. These techniques are employed in response to the increasing demand for methods that allow the extraction process to be automated, extraction times to be shortened, the consumption of solvents to be reduced, and the exposure of operative personnel to solvents to be minimised.…”

Experimental design optimization for screening relevant free phenolic acids from various preparations used in Burkina Faso folk medicine

“…This procedure is overly expensive due to both the time involved and the potential product wasted in the many experiments that must be performed to find acceptable, though not necessarily optimal, operating conditions. Experimental design methodologies, more practical and efficient, have been reported as a suitable tool to optimize HPLC separations (Karnka et al, 2002;Onjia et al, 2002;Klein and Rivera, 2000). It involves a statistical design of experiments, which uniformly samples the experimental domain to generate an experimental test matrix.…”