Supercritical fluid extraction of all-trans-lycopene from tomato

A procedure is proposed for the supercritical fluid extraction of all-trans-lycopene from tomato using carbon dioxide at 40 degrees C without modifier. The present method minimizes the risk of degradation via isomerization and oxidation of health-promoting ingredients, such as lycopene. The effect of different experimental variables on the solvating power of the supercritical fluid was evaluated in terms of both the selectivity achievable in the process and the yield of the extraction of all-trans-lycopene. Satisfactory separations of the all-trans-lycopene isomers from the cis counterparts were achieved using a C(30) column. The obtained extract contained 88% all-trans-lycopene and 12% cis-lycopene.     

Supercritical fluid extraction of alkylamides from Echinacea angustifolia

Echinacea has been known for its immunostimulatory activity, and its alkylamide components have been linked to such biological activity. Consequently, alkylamides in Echinacea angustifolia were extracted using supercritical carbon dioxide from fresh and dried roots at 45-60 degrees C and 34-55 MPa, and the alkylamide yield in the extracts was determined. The yield of alkylamides from fresh roots increased with temperature yet decreased with pressure, whereas the yield from air-dried roots (moisture content 8.4%) increased with both temperature and pressure. Freeze-drying of the roots to a moisture content of 4.9% did not result in any further increase in the yield compared to that of air-dried roots. Alkylamide yield of the ground dried roots extract was the highest (p < or = 0.05) among those from fresh, ground and unground E. angustifolia roots. Supercritical fluid extraction therefore shows potential for the recovery of alkylamides from dried Echinacea roots.     

Supercritical fluid extraction of lycopene from tomato processing byproducts

Tomato seeds and skins acquired from the byproduct of a local tomato processing facility were studied for supercritical fluid extraction (SFE) of phytochemicals. The extracts were analyzed for lycopene, beta-carotene, alpha-carotene, alpha-tocopherol, gamma-tocopherol, and delta-tocopherol content using high-performance liquid chromatography-electrochemical detection and compared to a chemically extracted control. SFEs were carried out using CO(2) at seven temperatures (32-86 degrees C) and six pressures (13.78-48.26 MPa). The effect of CO(2) flow rate and volume also was investigated. The results indicated that the percentage of lycopene extracted increased with elevated temperature and pressure until a maximum recovery of 38.8% was reached at 86 degrees C and 34.47 MPa, after which the amount of lycopene extracted decreased. Conditions for the optimum extraction of lycopene from 3 g of raw material were determined to be 86 degrees C, 34.47 MPa, and 500 mL of CO(2) at a flow rate of 2.5 mL/min. These conditions resulted in the extraction of 61.0% of the lycopene (7.19 microg lycopene/g).     

Analysis of limonoid glucosides from citrus by electrospray ionization liquid chromatography-mass spectrometry

An electrospray ionization liquid chromatography-mass spectrometry (ESI-LC-MS) method for the detection and quantitation of limonoid glucosides has been developed. Negative ions [M - H(+)](-) characteristic of six limonoid glucosides can be detected and quantified from selected ion monitoring chromatograms using carminic acid as an internal standard. The described method has been applied to the analysis of limonoid glucoside content in various liquid and solid Citrus spp. samples as well as complex mixtures of partially purified limonoid glucosides. Rapid and sensitive qualitative screening of samples for limonoid glucosides can also be accomplished with slight modifications of the method.     

Supercritical fluid extraction of 2,4,6-trichloroanisole from cork stoppers

2,4,6-Trichloroanisole (TCA) is the compound most often associated with cork taint in wines and has been shown to have a very low sensory threshold ( approximately 5 ng/L in wine). A supercritical fluid extraction (SFE) method for TCA in bark cork stoppers was developed with quantification via gas chromatography-mass spectrometry with selected ion monitoring. Supercritical carbon dioxide functioned as the extracting solvent, and temperature and pressure were optimized for the extraction. The method was validated using the stable isotope (2)H(5)-TCA as the internal standard. Recovery of TCA from spiked corks was found to be within 1-4% of the theoretical concentration with a coefficient of variation ranging from 2.6 to 9.7%. TCA levels in corks pulled from wines described as tainted by experienced judges ranged from 0.13 to 2.11 microg/g of cork. The SFE procedure offers a rapid, quantitative, nearly solvent-free, and automated method for the extraction of TCA from complex solid matrices such as cork.     

Supercritical fluid extraction of grape glycosides

Supercritical fluid extraction with methanol-modified CO(2) was used to extract glycosides from grapes. An optimization design involving 12 extraction variables was applied to achieve quantitative recoveries. The most important factor was the amount of organic modifier, a consequence of the high degree of glycoside polarity. By the proposed method, the total time of analysis can be decreased relative to that required for more conventional extractions. The full method can also be automated.     

Supercritical fluid extraction of 5-hydroxymethyl-2-furaldehyde from raisins

An extraction method based on supercritical CO(2) has been developed for the analysis of 5-hydroxymethyl-2-furaldehyde in raisins. To optimize extraction variables, a fractional factorial experimental design was applied. Six extraction variables were optimized. The organic modifier used for increasing the extraction fluid solvating power was the most important factor. Methanol as organic modifier produced 10-fold higher recoveries of 5-hydroxymethyl-2-furaldehyde than ethyl acetate. The efficiency of the organic modifier in the static extraction phase was compared with using it in the dynamic extraction phase. Repeatability of the analysis method was evaluated, which resulted in an RSD of <5%. 5-Hydroxymethyl-2-furaldehyde was quantified in raisins, and the concentration was found to be 0.128 mg/g of raisin.     

超临界CO2流体萃取槟榔中的槟榔碱

为了优化超临界CO2萃取槟榔碱的工艺参数,通过三元二次通用旋转组合设计实施试验,考察了萃取温度、萃取压力和萃取时间因素对槟榔碱萃取量的影响.试验结果表明:超临界萃取的温度对槟榔碱萃取量有极显著的影响,萃取时间和压力的影响较小.同时确定了槟榔碱萃取的最佳工艺参数为萃取温度72°C,压力57 MPa,时间26 min.在此条件下,槟榔碱的萃取量为6143.71/μg/g,达到理论最大萃取量的95.3%,所得萃取物中槟榔碱的百分含量晕为(25.85±0.41)%.     

Supercritical fluid extraction of organochlorine pesticides in eggs

The efficacy of supercritical fluid extraction (SFE) for the recovery of 16 common organochlorine pesticides (OCPs) from liquid whole eggs was investigated by employing supercritical carbon dioxide (SC-CO(2)) without the use of a solvent modifier to minimize interfering coextractives. The OCPs tested included aldrin; alpha-, beta-, delta-, and gamma-BHCs; p,p'-DDD, -DDE, and -DDT; dieldrin; endosulfans I, II, and sulfate; endrin; endrin aldehyde; heptachlor; and heptachlor epoxide. The SFE conditions were as follows: 10000 psi (680 bar), 40 degrees C, SC-CO(2) flow rate of 3.0 L/min with an extraction time of 40 min for a total of 120 L of CO(2). The OCPs were trapped off-line in an SPE cartridge containing Florisil and then eluted by an acetone/hexane mixture and analyzed by gas chromatography-electron capture detection (GC-ECD). Recovery studies were carried out on homogenized eggs fortified at the 0.05, 0.10, and 0.20 ppm levels. At the lowest level, 0.05 ppm, recoveries ranged from 81.8 to 108.3%, with CVs < 9.8%. All recoveries were significantly higher than those obtained by an AOAC/FDA solvent extraction method. Eggs containing incurred endosulfan I were also effectively extracted by SFE. This study suggests that the application of SFE for the extraction of OCPs from eggs will result in significant savings in analysis time and lower solvent use and disposal costs compared to conventional solvent extraction procedures.     

柚皮中柚皮苷乙醇提取工艺研究

该文采用乙醇浸提法从柚皮中提取柚皮苷,在单因素试验的基础上用正交试验进行工艺参数的优化,其适合的工艺条件为：提取温度60℃,提取时间90 min,提取液乙醇浓度50%,液料比25∶1(v/w),在此工艺条件下进行试验,柚皮苷提取率为91.784%。     

超临界CO2流体萃取槟榔中的槟榔碱

为了优化超临界CO₂萃取槟榔碱的工艺参数,通过三元二次通用旋转组合设计实施试验,考察了萃取温度、萃取压力和萃取时间因素对槟榔碱萃取量的影响。试验结果表明：超临界萃取的温度对槟榔碱萃取量有极显著的影响,萃取时间和压力的影响较小。同时确定了槟榔碱萃取的最佳工艺参数为萃取温度72℃,压力57 MPa,时间26 min。在此条件下,槟榔碱的萃取量为6143.71 μg/g,达到理论最大萃取量的95.3%,所得萃取物中槟榔碱的百分含量为（25.85± 0.41）% 。     

Supercritical fluid extraction of the pesticides carbosulfan and imidacloprid from process dust waste

Large amounts of contaminated process dust remain from the procedure of pesticide treatments applied to seed pellets. A pilot study in analytical-scale supercritical fluid extraction (SFE) was performed to determine the possibility of using supercritical carbon dioxide for the extraction of the nonpolar insecticide carbosulfan and the more polar insecticide imidacloprid present in contaminated dust waste, at concentrations of up to 20% (w/w). The effects of various experimental conditions, such as temperature, flow rate, and addition of modifier, on the recovery of the analytes were evaluated by extracting the pesticides both from spiked support material and from real dust samples. It was found that carbosulfan could easily be extracted from the dust waste within 30 min at 138 bar and 40 degrees C with a recovery of 98.9% (RSD = 2.3%, n = 10), compared to values obtained with a validated liquid extraction method. A sufficient removal of the more polar substance imidacloprid required the addition of a modifier, and the results showed a strong dependence of the extraction efficiency on the choice of modifier. Extractions at 276 bar and 80 degrees C with a solvent consisting of supercritical carbon dioxide modified with methanol (5%) gave a recovery of 97.0% (RSD = 3.6%, n = 10) using a 40 min extraction time. The results indicate that it seems to be possible to use process-scale SFE for the decontamination of pesticides from dust waste. The conditions outlined also permit analytical determinations of the two insecticides based on a combination of SFE and liquid chromatography.     

Supercritical fluid extraction of atrazine and other triazine herbicides from fortified and incurred eggs

Triazines are a class of important pre-emergent weed herbicides. Some members of this class of herbicides exhibit carcinogenic and immunotoxicity properties, which make their use controversial in areas where animal feed crops are grown. It is therefore important to determine if triazine residues are transported to animal food products in order to ascertain the extent of human exposure. Most of the current herbicide residue extraction methods are time-consuming and solvent intensive. Supercritical fluid extraction (SFE) using CO(2) has been used as a alternative for other residue extraction methods as a replacement for hazardous organic solvents. In this study, 10 triazines were extracted from eggs fortified at 100 ppb using unmodified supercritical CO(2) at a pressure of 10000 psi and a temperature of 50 degrees C with off-line collection on a solid phase extraction cartridge containing Florisil. Atrazine recovery averaged 90.4% with an RSD of 3.3%. The other triazines were recovered at mean levels >73%. In a separate feeding study, atrazine and two of its dealkyl metabolites were detected in the egg. The results indicate that SFE is a viable technique for isolating triazine residues from eggs, requiring only 8 mL of solvent for each analysis.     

Supercritical fluid extraction and fractionation of different preprocessed rosemary plants

Two-step supercritical fluid extraction of rosemary leaves at selected conditions of pressure and temperature is proposed to divide the oleoresin into two fractions with different antioxidant activities and essential oil compositions. Rosemary leaves obtained from different sources have been extracted and evaluated in terms of antioxidant activity and essential oil yield and composition. Also, a new device is proposed to improve the performance of the technique in terms of sample collection after SFE.     

Supercritical fluid extraction of pesticides from a table-ready food composite of plant origin (gazpacho)

Supercritical fluid carbon dioxide extraction (SFE) has been evaluated for the extraction of 17 organohalogen and organophosphate pesticides in gazpacho (a table-ready food composite containing crude vegetables, white bread, vegetable oil, water, and other minor components) using anhydrous magnesium sulfate as drying agent. The effects of different parameters, such as fat content in gazpacho composites, magnesium sulfate/gazpacho ratio, supercritical fluid volume, pressure, temperature, and static modifier additions, on SFE recoveries from spiked gazpacho samples have been studied. Analyses were performed by gas chromatography (GC) with flame photometric (FPD), electron capture (ECD), and mass spectrometry (MSD) detectors. In most experiments, recoveries obtained for the nonpolar organohalogen pesticides were lower than those obtained for the most polar organophosphate pesticides, but overall pesticide recoveries determined by using the optimal SFE conditions indicate that SFE could be used to determine pesticide residue levels in gazpacho.     

Supercritical fluid extraction of bioavailable amino acids from soils and their liquid chromatographic determination with fluorometric detection

A new procedure with supercritical CO2 modified with 0.5 mL of water and 0.75 mL of 0.1 M HCl in situ and 0.75 mL of water on-line at 15 MPa and 50 degrees C for 45 min was applied for the extraction of bioavailable amino acids from soil samples. Total extraction time was 60 min, but more favorable conditions are even possible for selected groups of amino acids. All analytes were trapped into 20 mL of methanol with satisfactory recovery (94-104%) and determined using high-performance liquid chromatography with fluorometric detection on a Zorbax Eclipse column (4.6 x 75 mm, 3.5 microm) with Na2HPO4 and acetonitrile/methanol/water as a mobile phase. Linear calibration curves were obtained (r > 0.999 except 0.99823 for Ile) with lower limits of detection (S/N = 3) in the range from 1.54 pg (Gly) to 13.5 pg (Cy2) or from 18.6 fmol (Ser) to 64.8 fmol (Lys). Validation and repeatability data are also given. Comparable results were obtained with a robust, commonly used extraction method (0.5 M ammonium acetate, 60 min in shaker, followed by filtration and lyophilization). Limiting values of artificial release of amino acids were also determined for each soil sample to eliminate any false results to ensure that all extracted amino acids originate from soil solution and exchangeable bound positions of soil samples.     

Supercritical fluid extraction of fat from ground beef: effects of water on gravimetric and GC-FAME fat determinations

This study investigated the supercritical carbon dioxide (SC-CO(2)) extraction of fat from ground beef and the effects of several factors on the gravimetric determination of fat. The use of ethanol modifier with the SC-CO(2) was not necessary for efficient fat extraction; however, the ethanol did increase the coextraction of water. This coextraction of water caused a significant overestimation of gravimetric fat. Oven-drying ground beef samples prior to extraction inhibited the subsequent extraction of fat, whereas oven-drying the extract after collection decreased the subsequent gas chromatographic fatty acid methyl ester (GC-FAME) fat determination. None of the drying agents tested were able to completely prevent the coextraction of water, and silica gel and molecular sieves inhibited the complete extraction of fat. Measurements of collection vial mass indicated that CO(2) extraction/collection causes an initial increase in mass due to the density of CO(2) (relative to displaced air) followed by a decrease in vial mass due to the removal of adsorbed water from the collection vial. Microwave-drying of the empty collection vials removes approximately 3 mg of adsorbed water, approximately 15-20 min is required for readsorption of the displaced water. For collection vials containing collected fat, microwave-drying effectively removed coextracted water, and the vials reached equilibration after approximately 10-15 min. Silanizing collection vials did not significantly affect weight loss during microwave-drying. SC-CO(2) can be used to accurately determine fat gravimetrically for ground beef, and the presented method can also be followed by GC-FAME analysis to provide specific fatty acid information as well.     

黑莓籽油的超临界萃取及脂肪酸成分分析

为了获得高品质保健油脂,采用超临界CO2萃取黑莓籽油,以气相色谱-质谱（GC-MS）对黑莓籽油脂肪酸成分进行分析。样品最佳粉碎粒度60目,超临界CO2萃取适宜工艺条件为：萃取压力20 MPa,分离罐压力10 MPa,萃取罐温度45℃,萃取时间30 min,萃取得率为(17.73±0.19)%。GC-MS检测结果显示黑莓籽油中含有丰富的不饱和脂肪酸,尤其是亚油酸、油酸、亚麻酸,质量分数分别为58.04%、11.76%、8.38%,占总脂肪酸的78.18%。研究结果为黑莓籽的综合开发加工利用提供了参考。     

超临界二氧化碳萃取蒜汁中大蒜油的研究

利用超临界二氧化碳对蒜汁中大蒜油的萃取进行了研究,结果表明：萃取釜中添加填料可以大大提高萃取速度;一次压榨汁大蒜素含量高,萃取速度快,但通过延长萃取时间,两次压榨汁可以得到较高的萃取率;超临界CO₂萃取蒜汁中大蒜油的最佳萃取条件为萃取压力15 MPa,萃取温度40℃,CO₂流量11 kg/h。该方法得到的大蒜油成分与从破碎大蒜固体中萃取得到的大蒜油成分基本相同,大蒜素含量在40%以上。     

柚子花芳香油超临界CO2萃取研究

介绍了新鲜柚子花中芳香性成分超临界CO2萃取分离工艺和分析检测方法,重点探讨了压力、温度、时间对萃取率的影响.应用正交试验优化得出:影响萃取的主次因素依次为为萃取压力、萃取温度、萃取时间;较佳工艺参数为:压力18MPa,温度50℃,时间90 min,流量25 L/min,得到超临界柚子花芳香油的萃取率高达2.7‰.应用气相色谱-质谱联用仪共鉴定出39个组分,占总芳香油的91.281%.通过对柚子花的深度加工研究,为开发高附加值的柚子花香精提供科学依据.