An optimal extraction method for the removal of templates from molecularly imprinted polymers (MIPs) is presented. The extraction method is based on pressurized hot water extraction (PHWE). PHWE was evaluated by application to three distinctly colored MIPs for chlorophyll (green), quercetin (yellow) and phthalocynine (dark blue) with subsequent monitoring of template removal and template bleeding by an ultraviolet spectrophotometer. The templates were washed-off and the extraction efficiency (EE) was compared to that of soxhlet and ultrasonic extraction methods. PHWE employed hot water at an optimal temperature of 220°C, pressure of 50 bars and flow rate of 2 mL min -1 to thoroughly wash-off the respective templates from their MIPs. The EE evaluated for PHWE was over 99.6% for all the MIPs with no subsequent or minimal template bleeding (\0.01%). The washing procedure was simple and relatively fast as it was achieved in 70 min at the most. At 95% confidence level (n = 3), soxhlet and ultrasonic recorded EE that was not significantly different (\94.5% in all cases) from that of PHWE ([99.6% in all cases). Soxhlet and ultrasonic had washing procedures that were slower (over 18 h) and employed large quantities (400 mL) of organic solvents modified with acids. The percentage relative standard deviations (%RSD) for the EE and recovery results were less than 2.3% in all cases indicating the high reproducibility of the method. Overall, the three methods performed comparably in extracting templates. PHWE seems to be the method of choice as it employed water which poses no environmental threat.
Electrospun polystyrene (PS) nanofibers (130-500 nm) incorporating a potassium salt of imidazole-1-carbodithioate were evaluated as potential sorbents for the pre-concentration of a model organochlorine pesticide; 1,1-dichloro-2,2bis-(4-chlorophenyl)ethylene (DDE). The efficiencies of DDE (0.25-1.0 lg L -1 ) adsorption by the nanofiber sorbent followed by desorption employing pressurized hot water extraction (PHWE) were investigated and monitored using gas chromatography with electron capture detection (GC-ECD). Parameters such as time, temperature and pressure of extraction, sample volume, DDE concentration and sorbent mass were optimized. The maximum adsorption of DDE (0.50 lg L -1 ) on electrospun PS and carbodithioate incorporated PS nanofibers was at 43.7 and 94.6%, respectively, in 20 min. Incorporation of carbodithiote doubled the adsorption efficiency of PS and achieved LOD of 0.000234 lg L -1 for DDE. The optimal DDE desorption on the PHWE system was 93.8% in 10 min. It would seem that the use of electrospun nanofibers as sorbent material with subsequent desorption by PHWE has great potential and thus warrants further investigations. This approach as it uses water as an extraction solvent for an organochlorine pesticide provides an opportunity to eliminate organic solvents, especially for procedures aimed at monitoring organic pollutants in the environment.
A quick, efficient and environmentally beneficial approach for the extraction of alkaloids in goldenseal based on pressurized hot water extraction (PHWE) is presented. PHWE was evaluated following the extraction of hydrastine and berberine which are the two main alkaloids of goldenseal. The effects of temperature and other parameters on extraction yields were monitored by high performance liquid chromatography coupled to diode array detector (HPLC-DAD). The extraction yields were compared to those achieved through reflux and ultrasonic extraction methods. PHWE employed hot water at an optimal temperature of 140˚C, a pressure of 50 bars and flow rate of 1 mL·min −1 for extraction experiments conducted in the dynamic mode. Both PHWE and conventional methods achieved comparable extraction yields. Reflux and ultrasonic extractions had procedures that were slower (over 6 h) and employed large quantities (200 mL) of organic solvents. The PHWE method was simple and relatively fast as extraction was achieved in 15 min. At 95% confidence level (n = 3), reflux and ultrasonic methods recorded extraction yields that were not significantly different from that of PHWE. Moreover, PHWE employed a more readily available "green" solvent, (water) to achieve comparable results to those of conventional methods which utilized organic solvents. The percentage relative standard deviations (%RSD) for the extraction yields were less than 3% in all cases indicating the high reproducibility of the method. However, when using PHWE to extract thermally labile analytes like alkaloids, degradation effects also occurred. Increasing the temperatures certainly achieved higher extraction yields but also led to degradation of these thermally labile compounds indicating a necessity for optimization.
A novel molecularly imprinted polymer (MIP) powder designed for the selective removal of interfering chlorophyll pigment from heavily pigmented green plant extracts during pesticide residue analysis or analysis for bioactives in natural product research is reported. The polymer powder imprinted with chlorophyll was synthesized by copolymerizing the functional and crosslinking monomers, methacrylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA), respectively. During batch rebinding experiments, the MIP effectively removed chlorophyll from neat chlorophyll standards, green medicinal plants, and spinach extracts with determined absorbance as high as 2.501 absorbance units (Au) to as low as 0.084 Au after the optimum quantity of the MIP (170 mg mL −1 ) was added as the adsorbent prior to instrumental analysis. The determined 0.084 Au absorbance was far below the absorbance of 2% chlorophyll (0.401 Au) regarded as the cut-off point for interfering chlorophyll. Thus the newly developed polymer presents itself as a suitable adsorbent for the selective removal of chlorophyll from heavily pigmented, chlorophyll containing extracts.
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