Preparation of supercritical fluid extraction using dry ice and exploration of equation of state to predict the operating conditions

Abstract Supercritical fluid extraction (SFE) of fruits and vegetables poses unique sample preparation considerations because the sample size is small (1–3 g) and the analyte is distributed in a moist solid matrix. The goal of this research was to develop practical sample preparation procedures for SFE of pesticide residues in produce so that acceptable accuracy and precision are maintained. In this study, 130 extractions of potato, fortified with up to 40 pesticides, were performed with 2 commercial SFE instruments. Extracts were analyzed by gas chromatography with ion trap mass spectrometry or electron capture detection. Four sample preparation procedures were tested and Hydromatrix was used to control the amount of water in the sample. The highest recoveries and lowest standard deviations were obtained when 20–50 g samples were blended with an equal amount of Hydromatrix and dry ice was added to keep the samples frozen. The dry ice helped produce a homogeneous flowable powder and greatly reduced the degradation or vaporization of several pesticides. Recoveries of most pesticides from subsamples of <4 g with this procedure were 90–105%, with relative standard deviations of 1–6%. Only diphenylamine and disulfo-ton gave reduced recoveries with this procedure. When samples were extracted sequentially with an autosampler, certain pesticides were degraded in the extraction vessels over a period of several hours. To avoid losses of these pesticides, the sample in the extraction vessel was either purged with CO2 to remove oxygen or kept frozen until extracted. Peach and orange check samples were analyzed with the method, and results were comparable with those from traditional analyses.

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Critical review of supercritical fluid extraction of selected spice plant materials

Macedonian Journal of Chemistry and Chemical Engineering ◽

10.20450/mjcce.2011.35 ◽

2011 ◽

Vol 30 (2) ◽

pp. 197 ◽

Cited By ~ 31

Author(s):

Milan N. Sovilj* ◽

Branislava G. Nikolovski ◽

Momčilo Đ. Spasojević

Keyword(s):

Supercritical Fluid Extraction ◽

Supercritical Fluid ◽

Flow Rate ◽

Operating Conditions ◽

Pharmaceutical Drugs ◽

Fluid Extraction ◽

Plant Materials ◽

Solvent Flow Rate ◽

Pharmaceutical Industries ◽

Solvent Flow

Supercritical fluid extraction (SFE) is one of the relatively new efficient separation method for the extraction of essential oils from different plant materials. The new products, extracts, can be used as a good base for the production of pharmaceutical drugs and additives in the perfume, cosmetic, and food industries. The aim of this work was to analyze the supercritical carbon dioxide extraction (SC-CO2) of oils from the selected spice plant materials. In this paper the process parameters such as pressure, temperature, solvent flow rate, size of grinding materials, and ratio of the co-solvent were presented for the selected spice plant materials: black pepper, caraway, celery, cinnamon, clove, coriander, daphne, fennel, ginger, hyssop, juniper, lavender, oregano, pennyroyal, red pepper, safflower, sage, turmeric, and vanilla. The values of operating conditions were: pressure from 7.5 to 68 MPa, temperature from 293 to 363 K, solvent flow rate from 0.003 to 30.0 kg/h, and diameter of grinding material from 0.17 to 3.90 mm. The global yield and quality of the extracts all of the plant material investigated, as well as the possibility of their application in the food, cosmetics and pharmaceutical industries were analyzed. The composition of the extracts was wery complex, and in every case the extract was composed of more than 200 components. All the compounds from the CO2 extracts were classified in the following groups: monoterpene, sesquiterpene, oxygenated monoterpene, and oxygenated sesquiterpene and other hydrocarbon groups. In some of the systems investigated the different mathematical models (Sovová, Hong), which have taken from the literature, were used to correlate the experimental data.

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Effect of Static Extraction Time on Supercritical Fluid Extraction of Bioactive Compounds from Phyllanthus niruri

Journal of Computational and Theoretical Nanoscience ◽

10.1166/jctn.2020.8742 ◽

2020 ◽

Vol 17 (2) ◽

pp. 918-924 ◽

Cited By ~ 1

Author(s):

Norsyamimi Hassim ◽

Masturah Markom ◽

Masli Irwan Rosli ◽

Shuhaida Harun

Keyword(s):

Supercritical Fluid Extraction ◽

Supercritical Fluid ◽

Bioactive Compounds ◽

Total Content ◽

Operating Conditions ◽

Extraction Time ◽

Fluid Extraction ◽

Active Components ◽

Phyllanthus Niruri ◽

Static Extraction

Supercritical fluid extraction (SFE) is an effective method to extract active components from plants. SFE process can be conducted by using a static or/and dynamic extraction. Static extraction is important for the diffusion of solvated analyte to the matrix surface. Therefore, the main objective of this study is to evaluate the static extraction time influence on SFE extraction of Phyllanthus niruri and the main bioactive compounds. The extraction was conducted by using supercritical carbon dioxide (SC-CO2) with 50% ethanol-water as a co-solvent at selected operating conditions (200 bar, 60 °C, 10% co-solvent content and 3 ml/min solvent total flow rate). The static extraction time was investigated in the range of 15 min–75 min by allowing the plant matrix to immerse in a mixture of SC-CO2 and 50% ethanol-water at the operating condition. The quantification of targeted compounds, which were gallic acid (GA), corilagin (CO) and ellagic acid (EA) were analysed by using high performance liquid chromatography (HPLC). The observation on the physical characteristics of the plant matrix was performed by using the scanning electron microscopy (SEM). The best result for total extraction yield was obtained at 60 min of static extraction time, which was 20.7% g/g sample. It also gave a better result for all three targeted compounds in terms of total content percentage (0.35% g GA/g extract, 3.05% g CO/g extract, and 5.17% g EA/g extract). In conclusion, static extraction time was crucial in extracting bioactive compounds in P. niruri by using SFE method and should be considered as the main parameter other than pressure and temperature.

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Scale-up approach for supercritical fluid extraction with ethanol–water modified carbon dioxide on Phyllanthus niruri for safe enriched herbal extracts

Scientific Reports ◽

10.1038/s41598-021-95222-0 ◽

2021 ◽

Vol 11 (1) ◽

Author(s):

Norsyamimi Hassim ◽

Masturah Markom ◽

Masli Irwan Rosli ◽

Shuhaida Harun

Keyword(s):

Carbon Dioxide ◽

Supercritical Fluid Extraction ◽

Supercritical Fluid ◽

Scale Up ◽

Operating Conditions ◽

Feed Ratio ◽

Fluid Extraction ◽

Phyllanthus Niruri ◽

Profitability Analysis ◽

Alcohol Water

AbstractScaling-up supercritical fluid extraction (SFE) for the extraction of bioactive compounds from herbal plants is challenging, especially with the presence of alcohol-water as co-solvent. Hence, the main objective of this study is to validate the scale-up criteria of SFE process for Phyllanthus niruri (P. niruri), and analyse the extract safety and profitability process at the industrial scale. The study was performed by using supercritical carbon dioxide (SC-CO2) with ethanol–water co-solvent at two operating conditions (L1: 200 bar, 60 °C and L2: 262 bar, 80 °C). The solvent-to-feed ratio (S/F) scale-up validation experiments were conducted at both operating conditions with feed mass capacity of 0.5 kg. The extraction yields and overall extraction curves obtained were almost similar to the predicted ones, with error of 5.13% and 14.2%, respectively. The safety of scale-up extract was evaluated by using a toxicity test against zebrafish embryo (FETT). The extract exhibited a low toxic effect with the LD50 value of 505.71 µg/mL. The economic evaluation using a detailed profitability analysis showed that the SFE of P. niruri was an economically feasible process, as it disclosed the encouraging values of return on investment (ROI) and net present values (NPV) for all scale-up capacities.

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