Microwave-assisted extraction (MAE) is widely employed in the analysis and the extraction of active compounds from plants. This review summarizes the research done during the last decade on the MAE of active ingredients from plants. Advances and modifications to improve the performance of MAE are presented and discussed in detail. Modified MAE such as vacuum microwave-assisted extraction (VMAE), nitrogen-protected microwave-assisted extraction (NPMAE), ultrasonic microwave-assisted extraction (UMAE), dynamic microwave-assisted extraction (DMAE) and other advancements in MAE are also detailed in this article. In addition, the microwave extraction procedures and the important parameters influencing its performance are also included, together with the advantages and the drawbacks of each MAE techniques.
Linusorbs (LO), cyclolinopeptides, are a group of cyclic hydrophobic peptides and considered a valuable by-product of flaxseed oil due to numerous health benefits. Currently applied acetone or methanol extraction could contaminate the feedstocks for further food-grade application. Using flaxseed cake as feedstock, this study established a practical method for preparing LO from pressed cake. Firstly, LO composition of 15 flaxseed cultivars was analyzed. Next, cold-pressed cake was milled and screened mechanically. The kernel and hull fractions were separated based on the disparity of their mechanical strength. Monitored by hyperspectral fluorescence, the LO-enriched kernel fraction separated from cold-pressed flaxseed cake was further used as feedstock for LO production. After ethanol extraction, partition, and precipitation, LOs were extracted from cold-pressed flaxseed cake with a purity of 91.4%. The proposed method could serve as feasible flaxseed cake valorization strategy and enable the preparation of other polar compounds such as flax lignan and mucilage.
The "ultrasonic-assisted extraction (UAE)" method was utilized in this work to assess how different process parameters affected the yield and recovery of phenolic compounds from the leaf of Commiphora gileadensis, which is one of the medicinal plants with a variety of biological functions. Its leaf is used for a various of therapeutic applications, such as the treatment of bacterial infections, inflammation, and wound healing. The "One-Factor-At-a-Time (OFAT)" approach was employed to examine the impacts of various UAE process parameters on the process of extraction, which include time of extraction, sample/solvent ratio, ultrasonic frequency, and solvent (ethanol) concentration. The extracts were then investigated for the presence of several phytochemicals using analytical techniques such as "Gas Chromatography-Mass Spectroscopy (GC-MS)" and "Fourier Transform Infrared Spectroscopy (FTIR)" studies. The findings showed that the maximum extraction yield, the total phenolic content (TPC), and the total flavonoids content (TFC) of the ethanolic extract of the leaves of C. gileadensis using the UAE method were at 31.80 ± 0.41 %, 96.55 ± 2.81 mg GAE/g d.w. and 31.66 ± 2.01 mg QE/g d.w. accordingly under a procedure duration of 15 min, ultrasonic frequency of 20 kHz, solvent/sample ratio of 1:20 g/mL, and solvent concentration of 40 % v/v. The leaves extract of C. gileadensis included 25 phenolic compounds that were previously unreported, and GC-MS analysis confirmed their presence. Hence, it follows that the UAE technique can successfully extract the phytochemicals from C. gileadensis for a variety of therapeutic uses.
This study optimized subcritical water extraction (SWE) conditions to maximize pectin yield from cocoa pod husk (CPH) and compared the characteristics of CPH pectin extracted through SWE with those of CPH pectin obtained through conventional extraction (CE) with citric acid. The Box-Behnken experimental design was employed to optimize SWE and examine the influence of process parameters, including temperature (100 °C-120 °C), extraction time (10-30 min), and solid:liquid ratio (SLR) (1:30-2:30 g/mL), on pectin yield. The maximum pectin yield of 6.58% was obtained under the optimal extraction conditions of 120 °C for 10 min with 1:15 g/mL SLR and closely corresponded with the predicted value of 7.29%. Compared with CE, SWE generated a higher yield and resulted in a higher degree of esterification, methoxyl content, and anhydrouronic acid value but a lower equivalent weight. The extracted pectin was pure, had low-methoxyl content, and similar melting and degradation temperatures.
Withania somnifera is an important medicinal plant traditionally used in the treatment of many diseases. The present study was carried out to characterize the phenolic acids, flavonoids and 1,1-diphenyl-2-picrylhydrazyl radical (DPPH) scavenging activities in methanolic extracts of W. somnifera fruits, roots and leaves (WSFEt, WSREt and WSLEt).
Six prenylated flavones, including one new compound, were isolated and identified from the stem bark extracts of Artocarpus altilis. The new prenylated flavone hydroxyartocarpin (1) was characterized as 3-(gamma,gamma-dimethylallyl)-6-isopentenyl-5,8,2',4'-tetrahydroxy-7-methoxyflavone and the known compounds were artocarpin (2), morusin (3), cycloartobiloxanthone (4), cycloartocarpin A (5) and artoindonesianin V (6). The structures of the compounds were determined by spectroscopic methods (IR, MS, (1)H-NMR and (13)C-NMR) and comparison with published data for the known compounds.
Dunaliine A (1), a new amino diketone, has been isolated from the leaves of Desmos dunalii together with four known dihydrochalcones: 2',4-dihydroxy-4',6'-dimethoxy-3',5'-dimethyldihydrochalcone (2), 2',4-dihydroxy-4',6'-dimethoxydihydrochalcone (3), 2',4-dihydroxy-4',5',6'-trimethoxydihydrochalcone (4) and 2',4-dihydroxy-5'-methyl-4',6'-dimethoxydihydrochalcone (5). The structures of these compounds were established notably by spectral analysis (1D- and 2D- (1)H, (13)C NMR), UV, IR and HRMS.
The present research was conducted to discover antimicrobial compounds in methanolic leaf extracts of Jatropha curcas and Andrographis paniculata and ethanolic leaf extract of Psidium guajava and the effectiveness against microbes on flower preservative solution of cut Mokara Red orchid flowers was evaluated. The leaves were analyzed using gas chromatography-mass spectrometry. A total of nine, 66, and 29 compounds were identified in J. curcas, P. guajava, and A. paniculata leaf extracts, with five (88.18%), four (34.66%), and three (50.47%) having unique antimicrobial compounds, respectively. The experimental design on vase life was conducted using a completely randomized design with 10 replications. The flower vase life was about 6 days in the solution containing the P. guajava and A. paniculata leaf extracts at 15 mg/L. Moreover, solution with leaf extracts of A. paniculata had the lowest bacterial count compared to P. guajava and J. curcas. Thus, these leaf extracts revealed the presence of relevant antimicrobial compounds. The leaf extracts have the potential as a cut flower solution to minimize microbial populations and extend flower vase life. However, the activities of specific antimicrobial compounds and double or triple combination leaf extracts to enhance the effectiveness to extend the vase life need to be tested.
Ultrasound-assisted extraction (UAE) with ethanol was used to extract the compounds responsible for the antioxidant activities of Misai Kucing (Orthosiphon stamineus). Response surface methodology (RSM) was used to optimize four independent variables: ethanol concentration (%), amplitude (%), duty cycle (W/s) and extraction time (min). Antioxidant compounds were determined by total phenolic content and total flavonoid content to be 1.4 g gallic acid equivalent/100 g DW and 45 g catechin equivalent/100 g DW, respectively. Antioxidant activities were evaluated using the 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS•+) radical scavenging capacity assay and the 2,2-diphenyl-1-picrylhydrazyl (DPPH•) radical scavenging capacity assay to be 1,961.3 and 2,423.3 µmol Trolox Equivalent Antioxidant Capacity (TEAC)/100 g DW, respectively. Based on the optimal conditions, experimental values were reported to be close to the predicted value by RSM modeling (p>0.05), indicating the suitability of UAE for extracting the antioxidants of Misai Kucing. Rosmarinic acid, kaempferol-rutinoside and sinesetine were identified by high performance liquid chromatography-mass spectrometry.
Policosanol, a mixture of long-chain alcohols found in animal and plant waxes, has several biological effects; however, it has a bioavailability of less than 10%. Therefore, there is a need to improve its bioavailability, and one of the ways of doing this is by nanoemulsion formulation. Different droplet size distributions are usually achieved when emulsions are formed, which solely depends on the preparation method used. Mostly, emulsions are intended for better delivery with maintenance of the characteristics and properties of the leading components. In this study, policosanol was extracted from rice bran wax, its composition was determined by gas chromatography mass spectrophotometry, nanoemulsion was made, and the physical stability characteristics were determined. The results showed that policosanol nanoemulsion has a nanosize particle distribution below 100 nm (92.56-94.52 nm), with optimum charge distribution (-55.8 to -45.12 mV), pH (6.79-6.92) and refractive index (1.50); these were monitored and found to be stable for 8 weeks. The stability of policosanol nanoemulsion confers the potential to withstand long storage times.
A rapid reversed-phase high performance liquid chromatographic method using a monolithic column for the determination of eight catechin monomers and caffeine was developed. Using a mobile phase of water:acetonitrile:methanol (83:6:11) at a flow rate of 1.4 mL min(-1), the catechins and caffeine were isocratically separated in about 7 min. The limits of detection and quantification were in the range of 0.11-0.29 and 0.33-0.87 mg L(-1), respectively. Satisfactory recoveries were obtained (94.2-105.2 ± 1.8%) for all samples when spiked at three concentrations (5, 40 and 70 mg L(-1)). In combination with microwave-assisted extraction (MAE), the method was applied to the determination of the catechins and caffeine in eleven tea samples (6 green, 3 black and 2 oolong teas). Relatively high levels of caffeine were found in black tea, but higher levels of the catechins, especially epigallocatechin gallate (EGCG) were found in green teas.
Different extraction conditions were applied to investigate the effect of temperature, extraction time and substrate-extractant ratio on pectin extraction from cocoa husks. Pectin was extracted from cocoa husks using water, citric acid at pH 2.5 or 4.0, or hydrochloric acid at pH 2.5 or 4.0. Temperature, extraction time and substrate-extractant ratio affected the yields, uronic acid contents, degrees of methylation (DM) and degrees of acetylation (DA) of the extracted pectins using the five extractants differently. The yields and uronic acid contents of the extracted pectins ranged from 3.38-7.62% to 31.19-65.20%, respectively. The DM and DA of the extracted pectins ranged from 7.17-57.86% to 1.01-3.48%, respectively. The highest yield of pectin (7.62%) was obtained using citric acid at pH 2.5 [1:25 (w/v)] at 95 °C for 3.0 h. The highest uronic acid content (65.20%) in the pectin was obtained using water [1:25 (w/v)] at 95 °C for 3.0 h.
A modeling technique based on absorbed microwave energy was proposed to model microwave-assisted extraction (MAE) of antioxidant compounds from cocoa (Theobroma cacao L.) leaves. By adapting suitable extraction model at the basis of microwave energy absorbed during extraction, the model can be developed to predict extraction profile of MAE at various microwave irradiation power (100-600 W) and solvent loading (100-300 ml). Verification with experimental data confirmed that the prediction was accurate in capturing the extraction profile of MAE (R-square value greater than 0.87). Besides, the predicted yields from the model showed good agreement with the experimental results with less than 10% deviation observed. Furthermore, suitable extraction times to ensure high extraction yield at various MAE conditions can be estimated based on absorbed microwave energy. The estimation is feasible as more than 85% of active compounds can be extracted when compared with the conventional extraction technique.
The ethyl acetate and methanol bark extracts of Melicope glabra were evaluated for their antioxidant capacities by 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radical scavenging activity and β-carotene bleaching/linoleic acid system. Both extracts exhibited strong inhibition against the DPPH radical (IC50 values of 24.81 and 13.01 μg ml(-1), respectively) and strong antioxidant activity in β-carotene bleaching assay. Both samples were found to have high phenolic content with values of 39 and 44 mg GAE/g as indicated by Follin-Ciocalteau's reagent. Antioxidant TLC assay-guided isolation on the methanol extract led to the isolation of a new pyranocoumarin, glabranin (1), umbelliferone (2), scopoletin (3) and sesamin (4), and their structures were determined by spectroscopy. Compounds (1-3) showed significant activities on DPPH free radical with the IC50 of 240.20, 810.02 and 413.19 μg ml(-1), respectively. However, in β-carotene bleaching assay, sesamin (4) showed higher inhibitory activity (1 mg ml(-1), 95%) than glabranin (1) (1 mg ml(-1), 74%), whilst umbelliferone (2) and scopoletin (3) were slightly pro-oxidant.
Solid phase extraction (SPE) using Sep-Pak® cartridges is one of the techniques used for fractionation of antioxidant compounds in waste of dabai oil extraction (defatted dabai parts). The aim of this study was to determine the phenolic compounds and antioxidant capacity in crude extracts and several SPE fractions from methanolic extract of defatted dabai pulp and peel. Based on SPE, Sep-Pak® cyanopropyl and C₁₈ cartridges were used to fractionate the antioxidant-rich crude extracts into water and methanolic fractions. Analyzed using LC-MS, flavonoids, anthocyanins, saponin derivatives and other unknown antioxidative compounds were detected in the defatted dabai crude extracts and their SPE fractions. Anthocyanins were the major phenolic compounds identified in the defatted dabai peel and detected in most of the SPE fractions. Methanolic fractions of defatted dabai parts embraced higher total phenolics and antioxidant capacity than water fractions. This finding also revealed the crude extracts of defatted dabai peel have the most significant antioxidant properties compared to the methanolic and water fractions studied. The crude extract of defatted dabai parts remain as the most potent antioxidant as it contains mixture of flavonoids, anthocyanins and other potential antioxidants.
Extraction and chromatographic separation of the extracts of dried stem barks of Glycosmis macrantha lead to isolation of two new acridone alkaloids, macranthanine and 7-hydroxynoracronycine, and a known acridone, atalaphyllidine. The structures of these alkaloids were determined by detailed spectral analysis and also by comparison with reported data.
The extracts of the stem bark of Calophyllum soulattri gave a new pyranocoumarin, soulamarin (1), together with five other xanthones caloxanthone B (2), caloxanthone C (3), macluraxanthone (4), trapezifolixanthone (5) and brasixanthone B (6) one common triterpene, friedelin (7), and the steroidal triterpene stigmasterol (8). The structures of these compounds were established based on spectral evidence (1D and 2D NMR).
Natural products from medicinal plants, either as pure compounds or as standardized extracts, provide unlimited opportunities for new drug leads because of the unmatched availability of chemical diversity. Due to an increasing demand for chemical diversity in screening programs, seeking therapeutic drugs from natural products, interest particularly in edible plants has grown throughout the world. Botanicals and herbal preparations for medicinal usage contain various types of bioactive compounds. The focus of this paper is on the analytical methodologies, which include the extraction, isolation and characterization of active ingredients in botanicals and herbal preparations. The common problems and key challenges in the extraction, isolation and characterization of active ingredients in botanicals and herbal preparations are discussed. As extraction is the most important step in the analysis of constituents present in botanicals and herbal preparations, the strengths and weaknesses of different extraction techniques are discussed. The analysis of bioactive compounds present in the plant extracts involving the applications of common phytochemical screening assays, chromatographic techniques such as HPLC and, TLC as well as non-chromatographic techniques such as immunoassay and Fourier Transform Infra Red (FTIR) are discussed.
To isolate Salmonella from curry samples and to evaluate the drug sensitivity of the food-borne Salmonella and its susceptibility to specific plant extracts.