Cloud point extraction of Δ9-tetrahydrocannabinol from cannabis resin.

A cloud point extraction coupled with high performance liquid chromatography (HPLC/UV) method was developed for the determination of Δ(9)-tetrahydrocannabinol (THC) in micellar phase. The nonionic surfactant "Dowfax 20B102" was used to extract and pre-concentrate THC from cannabis resin, prior to its determination with a HPLC-UV system (diode array detector) with isocratic elution. The parameters and variables affecting the extraction were investigated. Under optimum conditions (1 wt.% Dowfax 20B102, 1 wt.% Na2SO4, T = 318 K, t = 30 min), this method yielded a quite satisfactory recovery rate (~81 %). The limit of detection was 0.04 µg mL(-1), and the relative standard deviation was less than 2 %. Compared with conventional solid-liquid extraction, this new method avoids the use of volatile organic solvents, therefore is environmentally safer.

Emulsification processes: on-line study by multiple light scattering measurements.

The use of ultrasound in various processes of the chemical industry has been a subject of research and development for many years. As regards in emulsification, apart from formulation variables, power is the most important parameter. Efficiency of emulsification processes may be followed and evaluated by measuring particle size distribution, which mainly governs the kinetic stability of such dispersions. Unfortunately, this kind of measurement must be performed at high dilution (low volume fraction of dispersed phase). The present work is devoted to the on-line study of ultrasound emulsification by means of a newly developed apparatus based on multiple light scattering, which allows us to determine average droplet diameter and its variations directly on concentrated media. The model system was an oil (kerosene)-in-water emulsion stabilized by a polyethoxylated sorbitan monostearate.

Mechanism of calcite crystal growth inhibition by the N-terminal undecapeptide of lithostathine.

Pancreatic juice is supersaturated with calcium carbonate. Calcite crystals therefore may occur, obstruct pancreatic ducts, and finally cause a lithiasis. Human lithostathine, a protein synthesized by the pancreas, inhibits the growth of calcite crystals by inducing a habit modification: the rhombohedral (10 14) usual habit is transformed into a needle-like habit through the (11 0) crystal form. A similar observation was made with the N-terminal undecapeptide (pE(1)R(11)) of lithostathine. We therefore aimed at discovering how peptides inhibit calcium salt crystal growth. We solved the complete x-ray structure of lithostathine, including the flexible N-terminal domain, at 1.3 A. Docking studies of pE(1)R(11) with the (10 14) and (11 0) faces through molecular dynamics simulation resulted in three successive steps. First, the undecapeptide progressively unfolded as it approached the calcite surface. Second, mobile lateral chains of amino acids made hydrogen bonds with the calcite surface. Last, electrostatic bonds between calcium ions and peptide bonds stabilized and anchored pE(1)R(11) on the crystal surface. pE(1)R(11)-calcite interaction was stronger with the (11 0) face than with the (10 14) face, confirming earlier experimental observations. Energy contributions showed that the peptide backbone governed the binding more than did the lateral chains. The ability of peptides to inhibit crystal growth is therefore essentially based on backbone flexibility.

Emulsification by ultrasound: drop size distribution and stability.

The aim of this work is to compare the oil-in-water emulsions produced by mechanical agitation (Ultra-Turrax, 10,000 rpm, P = 170 W) or power ultrasound (ultrasound horn, 20 kHz, 130 W) using the same model system: water/kerosene/polyethoxylated (20 EO) sorbitan monostearate. The following parameters were varied: emulsification time, surfactant concentration, consumed power and volume fraction of oil. With ultrasound, the drop size (Sauter diameter, d32) is much smaller than that given by mechanical agitation under the same conditions, which makes insonated emulsions more stable. For a given drop size (d32), less surfactant is required.