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Proceeding Paper

Utilization of Ultrasonic-Assisted Extraction for Bioactive Compounds from Floral Sources †

1
Nutrition and Bromatology Group, Department of Analytical Chemistry and Food Science, Instituto de Agroecoloxía e Alimentación (IAA)—CITEXVI, Universidade de Vigo, 36310 Vigo, Spain
2
REQUIMTE/LAQV, Department of Chemical Sciences, Faculty of Pharmacy, University of Porto, R. Jorge Viterbo Ferreira 228, 4050-313 Porto, Portugal
*
Authors to whom correspondence should be addressed.
Presented at the 5th International Electronic Conference on Foods, 28–30 October 2024; Available online: https://sciforum.net/event/Foods2024.
Biol. Life Sci. Forum 2024, 40(1), 15; https://doi.org/10.3390/blsf2024040015
Published: 21 January 2025
(This article belongs to the Proceedings of The 5th International Electronic Conference on Foods)

Abstract

:
This systematic review aims to evaluate the effectiveness of ultrasound-assisted extraction (UAE) for obtaining bioactive compounds from floral sources, emphasizing its potential application in the pharmaceutical and food industries. As a “green extraction” technique, UAE minimizes use of organic solvents, energy consumption, and extraction time, making it a sustainable alternative to traditional extraction methods. On the other hand, flowers serve as a valuable reservoir of bioactive compounds. Appropriate experimental strategies are necessary to maximize the yield of bioactive compound recovery. The increasing use of floral sources in manufacturing dietary supplements and functional foods, coupled with rapid advancements in these sectors, indicates significant potential for the application of UAE. Its effectiveness is influenced by a multitude of factors, including operational variables and the matrix effect, both of which have the potential to impact the molecular structures of the specific compounds being targeted. In flowers, these compounds usually entail active secondary metabolites such as polyphenols. Hence, it is imperative to establish the optimal experimental parameters. A comprehensive literature review was conducted, covering studies from 2000 to 2024. Electronic databases including PubMed, ScienceDirect, Web of Science, and Scopus were searched for peer-reviewed articles using keywords such as “Ultrasound-assisted extraction”, “bioactive compounds”, “flowers”, and “extraction optimization”. Results indicate that UAE significantly enhances the yield of bioactive compounds, such as polyphenols, with extraction efficiencies reaching up to 95% under optimal conditions. The findings also highlight the importance of parameter optimization, as variations in solvent concentration and ultrasonic intensity can affect the structural integrity of extracted compounds. In conclusion, this communication has emphasized the significance of UAE technologies and presented recent research and updated data on their contribution to obtaining bioactive compounds from plant-based materials, particularly flowers.

1. Introduction

Bioactive compounds from natural sources, including flowers, have seen a surge in their popularity in recent years. These compounds include phenolic acids, flavonoids, alkaloids, stilbenes, saponins, terpenoids, and carotenoids from plant matrices (both whole plant and by-products) [1], which possess antioxidant, anti-inflammatory, and other health-promoting properties [2,3]. These have potential applications in the pharmaceutical, food, and cosmetic industries.
Traditional extraction methods, while effective, often require a large amount of energy, use of organic solvents, high temperatures, and long processing times, which can negatively impact these heat-sensitive compounds [4]. Therefore, ultrasound-assisted extraction (UAE) has emerged as a promising “green” alternative to conventional extraction techniques. UAE utilizes ultrasonic waves to create cavitation bubbles, which enhance cell wall disruption, allowing for an easier release of the bioactive compound into the extraction solvent [5]. The technique requires a low energy input and often operates under mild conditions, using short times and low temperatures. This allows for the preservation of the thermolabile bioactive compounds present in the flower matrix [5]. Optimization of UAE parameters is crucial for efficient extraction, maximizing the yield while preserving the structural integrity and activity of bioactive compounds. These parameters include ultrasonic power, frequency, extraction temperature, solvent concentration, and extraction time [6]. Often, advanced statistical and computational techniques like response surface methodology (RSM) and artificial neural networks coupled with genetic algorithms (ANN-GA) are employed to this effect [7]. The application of optimization techniques has not only been shown to improve extraction efficiency, but also reduce operational costs and minimize environmental impact.
This article provides a short review of the current research on UAE for bioactive compound extraction from flowers, exploring the benefits, challenges, and future potential of this technique in various industries (Figure 1).

2. Materials and Methods

To investigate bioactive compounds in floral sources through UAE extraction, a comprehensive systematic review was designed to conduct a review of reliable databases and high-impact journals. An extensive search was conducted across multiple platforms, including PubMed, Scopus, ScienceDirect, Web of Science, and Google Scholar, focusing on UAE, polyphenols, bioactive compounds, flowers, and extraction optimization. The research applied specific inclusion criteria, with a particular emphasis on works published between 2000 and 2024. The relevance of articles categorized in the first (Q1) and second (Q2) quartiles was prioritized to secure the inclusion of reliable data and high-quality research. Relevant studies were evaluated for utilizing optimization methods for ultrasonic extraction factors.

3. Ultrasound-Assisted Extraction (UAE) in Bioactive Compound Extraction

UAE is a method based on the phenomenon of cavitation that occurs in a solvent when high intensity waves pass through [1,8]. It is considered an innovative and green technology, as it is efficient and environmentally friendly compared to traditional extraction methods. UAE operates by producing cavitation bubbles that break down cell walls, improve solvent penetration, and accelerate the release of organic compounds from plant cells, increasing mass transfer across cell membranes [5,9]. The efficiency of the extractions depends on several process variables, such as ultrasonic power, frequency, extraction temperature, and solvent–sample interaction [6].
The extraction of bioactive compounds can be effectively increased using UAE, as it has been reported to increase the yield and rate of extraction of bioactive compounds [10], often achieving the highest extraction rates within the first few minutes [6]. Moreover, UAE reduces solvent and energy consumption, operational costs, and environmental footprint [11]. Its operation at moderate temperatures also assures that heat-sensitive compounds are minimally degraded [4].
UAE is also praised for its versatility, as it can be applied to various materials, including proteins, polysaccharides, and oils [12]. It has also been shown to work on complex matrices such as marine sediments and mussel tissue [13].
UAE has been applied to a great variety of flowers to extract bioactive compounds, including cotton, feijoa, pomegranate, tea, Jatropha integerrima, Amaranthus caudatus, Limonium sinuatum, chamomile, and chestnut flowers. In a study on cotton flowers, UAE extracted the highest amounts of polyphenols (214.07 mg/g) and flavonoids (33.23 mg/g) of the tested methods [14]. Similarly, in a study of targeted flavonoids from edible feijoa (Acca sellowiana (O.Berg) Burret) flowers, UAE gave the highest yields for isoquercitrin, quercetin, total polyphenol content, and antioxidant activity [15]. Dong-ping Xu et al. applied a 7 min long UAE extraction to Jatropha integerrima flowers, yielding 1103.38 µmol Trolox/g DW of antioxidants, higher than traditional methods [16]. UAE can also extract pigments from flowers, as shown by Roriz et al., who effectively extracted betacyanin from Amaranthus caudatus flowers [17].
Optimizing UAE extractions for the targeted compounds is critical for its effectiveness, low cost, and low environmental impact [3]. Optimizing UAE extraction of Origanum majorana L. using response surface methodology significantly increased antioxidant activity and polyphenol content [18]. Advanced optimization techniques, such as the response surface methodology, can be coupled with more advanced techniques, such as an artificial neural network associated with a genetic algorithm (RSM-ANN-GA), providing better predictability and greater accuracy in determining optimal conditions [7]. Other techniques, such as natural deep eutectic solvents, can also be used in tandem, which effectively increases the curcuminoid extraction yield from Curcuma longa, Curcuma xanthorrhiza, and Curcuma mangga [19].
Using UAE to extract active ingredients from plants creates cavitation and positive mechanical effects [8]. UAE is a highly efficient, eco-friendly method for extracting bioactive compounds from various biological materials, including flowers. Optimization techniques, such as response surface methodologies, must be employed to ensure an effective extraction. This makes UAE an adaptable and promising tool for the sustainable extraction of valuable bioactive compounds across industries.

4. Floral Sources as a Reservoir of Bioactive Compounds

Flowers have gathered interest recently due to their rich content of bioactive compounds, which have the potential to offer various health benefits. These compounds include phenolics, flavonoids, and vitamins exhibiting antioxidant, antibacterial, and other properties [20].
Polyphenols and flavonoids are some of flowers’ most common bioactive compounds. These compounds often show potent antioxidant, anti-inflammatory, and antimicrobial properties. Fourteen commonly consumed flowers in China have been shown to contain many phenolic acids and flavonoids connected to their positive health effects on chronic diseases such as cancer, inflammation, and diabetes [2]. These bioactive compounds included a very high amount of gallic acid, protocatechuic acid, p-hydroxybenzoic acid, quercetin, hesperidin, and luteolin [2]. The polyphenol-rich water extract of the Dimocarpus longans Lour. flower has been shown to have anti-obesity and hypolipidemic effects in rats consuming a hypercaloric diet [21]. Polyphenols from the flower of Hibiscus syriacus exhibit neuroprotective effects and can ameliorate neuroinflammation [22]. Long-term consumption of a polyphenol-rich diet protects against cancers, cardiovascular diseases, diabetes, osteoporosis, and neurodegenerative diseases [23], and flower polyphenols can be an essential addition to this diet.
Flowers are also rich in pigments such as anthocyanins and betalains, which are known for their antioxidant and anticancer properties [20]. They can also be used as natural dyes due to their vibrant colors. Anthocyanins in edible flowers have long been considered a good candidate for extracting natural additives for use in the food industry as preservatives and colorants [24]. Anthocyanins are classified as flavonoids. Their consumption is associated with reducing oxidative stress and inflammation in the human body, as well as protective effects against cardiovascular diseases and neuroprotective effects. Łysiak et al. have noted that several commonly used ornamental flowers contain a significant presence of anthocyanins, which can enrich the human diet through their potent antioxidant and anti-inflammatory properties. Betalains are a rarer pigment found almost exclusively in the Caryophyllales order [25].
Similarly, they show several health benefits. For example, betalains from Portulaca grandiflora flowers show antioxidant activity, antibacterial activity, and anticancer selectivity toward colon carcinoma cells [26]. Furthermore, betalains have been shown to induce phase II enzymes’ antioxidant defense mechanisms and possibly prevent LDL oxidation and DNA damage [27]. Additionally, a review concluded that incorporating betalains from flowers into the human diet can have anti-inflammatory, cognitive impairment, anticancer, anti-hepatitis, and antidiabetic effects [28].
Vitamins and tocopherols can also be obtained from flowers, exhibit antioxidant properties, and can be used in cosmetic products. Edible flowers, such as apricot flowers, Celosia cristata, and various species from Yunnan Province, China, are rich in vitamins (pre-vitamin A, B-complex, C, and E), exhibiting strong antioxidant capacities [29]. In the case of borage, camellia, Centaurea, and pansy flowers, vitamin E, β-tocopherol, is the major vitamer [30]. Vitamin E is known for its antioxidant properties, which help prevent lipoprotein oxidation and inhibit platelet aggregation, potentially reducing cardiovascular disease (CVD) risk [31]. Vitamin E is also widely applied in cosmetics, acting as a major antioxidant in the skin, protecting it from oxidative stress, photoaging caused by UV radiation, and other environmental factors [32]. Vitamin C in flowers significantly contributes to their antioxidant activity. Apul et al. prepared an instant drink made from red seed guava and rosella flowers, which can be used as a source of vitamin C, showing a practical application of flowers in the food industry [33]. A significant amount of retinol activity equivalents have been measured in some flowers, such as Renealmia alpinia and Lantana camara, suggesting a potential use as a cosmetic ingredient [34]. Some flowers have also been reported to contain B-complex vitamins, such as Celosia cristata flowers, contributing to their nutritional and potential nutraceutical value [35].
Essential oils from certain flowers, such as chamomile and rose, contain many terpenoids. Terpenoids are already widely used in producing pharmaceuticals, flavors, fragrances, pesticides, and disinfectants [36]. For example, rose-scented geranium essential oil, rich in terpenoids, is highly valued in the perfumery industry for its fragrance [37]. These compounds also have health-promoting effects, with terpenoids present in herbal and dietary plants that are shown to help manage obesity-induced metabolic disorders like type 2 diabetes, hyperlipidemia, insulin resistance, and cardiovascular diseases [38]. Additionally, the terpenoid-based compound artemisin is widely recognized as an effective antimalarial drug, with artemisinin-based combination therapies (ACTs) currently the most effective treatment for malaria [39]. Monoterpenoids such as iridoids are an important class of compounds which is found in Verbascum sinuatum flowers. Harpagoside is one of the most abundant iridoids in Verbascum sinuatum flowers, with other identified compounds including catalposide, verbascoside, genipin, catalopl, and aucubin. These compounds have a significant role in antibacterial and antioxidant activity [40,41]. Beyond these compounds, Citrus aurantium L. flowers contain alkaloids, naturally occurring compounds. The presence of these bioactive secondary metabolites has been shown to lead to significant antimicrobial activity [42].
Flowers have emerged as valuable sources of bioactive compounds with significant health-promoting potential due to their considerable content of polyphenols, flavonoids, vitamins, and pigments such as anthocyanins and betalains. Flowers’ bioactive components have versatility and potential as natural additives in the food, cosmetic, and health industries.

5. Factors Influencing UAE Efficiency: Operational Variables, Matrix Effect

Design of Experiments (DOE) is a multi-variate mathematical-statistical methodology that rationally and efficiently explores the response of a system by connecting levels of variables that interact with it through an experimental matrix [43]. When combined with response surface methodology (RSM), DOE lets users manage data efficiently, build models of system behavior, analyze the interactions between factors, and determine the optimal region of the factor levels for predicting and optimizing experimental conditions [44,45]. As such, they are widely used in the field of optimization and modeling of bioactive compound extraction processes [44]. Application involves steps such as design, execution, evaluation, and validation of experimental results [46,47].
In the scope of UAE processes, factors such as the extraction process itself, the selected solvent, extraction time, solvent/solid ratio, season, location of harvesting, amplitude, duty cycle of ultrasonication, pH, frequency and power of the ultrasounds, particle size, and temperature are usually responsible for the efficiency of UAE, so these factors should be considered when performing DOE [1,8,48]. Operating variables such as frequency, amplitude, and ultrasonic power also matter, as they can influence the molecular structures and recovery of the target compounds, and therefore their biological properties [3]. To achieve maximum yield, a statistical analysis is desirable to ascertain the optimum condition for UAE, e.g., the Plackett–Burman design is used since it can minimize the non-significant variables in the models. Following this screening, important parameters should be selected for subsequent optimization of the process [49]. Additional experimental designs routinely used in UAE processes are the Box–Behnken, rotating composite central composite, Taguchi, D-optimal, fractional factorial, and Doehlert designs [9,49,50]. Two-level (22) and three-level (32) full factorial designs have been used, but in a small number of cases [1].
As acoustic cavitation is the basis of UAE, there is little doubt that the amplitude of the ultrasonic waves is a driving factor in its intensity. Regardless of optimization, elevated amplitudes have been proven to induce more vigorous cavitation phenomena, facilitating greater disruption of cellular structures and potentially magnifying the extraction efficiency. Nonetheless, excessively high amplitudes can also cause high temperatures within the matrices, thus diminishing the cavitation efficiency of the UAE process. An increase in the penetration power of the solvent and the contact surface of the solid and the solvent are the other effects of ultrasonic waves effects [51]. Moreover, it has been reported that the application of elevated temperatures generally leads to an increase in diffusion rate and solubility. However, the highest degradation rate of bioactive compounds such as phenolics can happen at very high extraction temperatures near 80 °C [52,53]. Free radical formation along with the alteration of conjugated double bonds in the compounds may result in fluctuations in radical scavenging. These variations can, in turn, impact the extraction yield of particular bioactive compounds throughout the extraction process [54].
For example, Hao et al., 2019 discussed critical factors influencing UAE. Their study optimized the UAE process to isolate phenolic compounds from Citrus aurantium L. flowers using Box–Behnken design. They reported that the key extraction factors were ethanol concentration, temperature, extraction time, and liquid-to-solid ratio [55]. Cai et al., 2022 emphasized that the interactive effects of several critical factors, analyzed using RSM, play a unique role in the UAE extraction process for alkaloids from flowers. Additionally, the floral matrix also effects solvent penetration and compound release [56].
As shown in Table 1, each of these tools has been successfully used to optimize the isolation of compounds including total polyphenols (TPC) and total antioxidants (TAA), obtaining high yields and antioxidant capacities, which demonstrates the robustness of these techniques.

6. Conclusions

While considerable improvements in yield have been achieved in numerous studies by optimizing extraction parameters, the task of establishing a universally effective method remains a challenge. There is no ideal extraction technique, since each method requires adaptation to the unique characteristics of the matrix and the target to be extracted. However, optimized UAE using models such as RSM has been successfully used to maximize the efficiency of extraction via UAE of herbal bioactive compounds. In the context of UAE uses, these tools simultaneously optimize efficiency while minimizing the degradation of sensitive bioactive compounds. Thus, UAE is an integrated strategy to ensure augmentation of the yield and stability of compounds isolated from floral sources, placing this high-speed, cost-effective and eco-friendly technique as a clear leader in I + D + i of products in the pharmaceutical, cosmetic, and food industries.

Author Contributions

Conceptualization, S.S.-M., M.C., and M.A.P.; methodology, S.S.-M., P.D., P.B., A.P.-V., F.C., and A.O.S.J.; validation, P.B., A.P.-V., F.C., and A.O.S.J.; formal analysis P.B. and A.O.S.J.; investigation, S.S.-M., P.D., P.B., A.P.-V., F.C., and A.O.S.J.; data curation, P.B., A.P.-V., F.C., and A.O.S.J.; writing—original draft preparation, S.S.-M., P.D., P.B., and A.O.S.J.; writing—review and editing, M.C. and M.A.P.; visualization, S.S.-M., P.B., A.O.S.J., and M.C.; supervision, F.C., M.C., and M.A.P.; project administration, M.C. and M.A.P.; funding acquisition, M.A.P. All authors have read and agreed to the published version of the manuscript.

Funding

The research leading to these results was supported by Xunta de Galicia for supporting the pre-doctoral grant of P. Barciela (ED481A-2024-230). The authors thank the EU-FORA Fellowship Program (EUBA-EFSA-2023-ENREL-01), which supports the work of F. Chamorro. The authors are grateful for the National funding by FCT, Foundation for Science and Technology, through the individual research grant A.O.S. Jorge (2023.00981.BD).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Data is contained within the article.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. Ultrasound-assisted extraction of bioactive compounds from floral sources: mechanism and benefits. Created with canva.com.
Figure 1. Ultrasound-assisted extraction of bioactive compounds from floral sources: mechanism and benefits. Created with canva.com.
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Table 1. Optimization of ultrasound-assisted extraction (UAE) with several experimental design methods.
Table 1. Optimization of ultrasound-assisted extraction (UAE) with several experimental design methods.
Opt. MethodTarget
Compounds
Solvent Conc. (%)S-to-s Ratio (mL/g)Temp. (°C)Time (min)R2Results/YieldsRef.
BBD + SVR-DATPC, TSC87.66%23 50260.99High antioxidant capacity; promising for pharma/cosmetics[50]
PBD + BBDPMF, DMF, TMF95%50 5015.990.97TMC = 327.25 mg/g[49]
Taguchi methodATC, TPC77.72–84104045ns.2.12 mg cy-3-glu/g dw (ATC), 6.67 mg gallic acid/g dw (TPC)[9]
D-optimalTPC, TAA76.97283014.220.997.19 mg/g dw (TPC), 88.36% DPPH (TAA)[48]
Two-level (22)TPC, TAA553630680.9772.7 mg gallic acid/g dw (TPC), 50.9 µmol TE/g DPPH dw (TAA)[44]
CCDTPC, TAA3.63.65630.964.34 mg/g (TPC), 73.5% (TAA)[51]
Abbreviations: TPC: Total Phenolic Content; TSC: Total Saponin Content; SVR-DA: Support Vector Regression with Dragonfly Algorithm; PBD: Plackett–Burman design; BBD: Box–Behnken design; PMF: 3,5,7,3?,4′-pentamethoxyflavone; DMF: 5,7-dimethoxyflavone; TMF: 5,7,4′-trimethoxyflavone (TMF); TMC: Total methoxyflavone content; ATC: Anthocyanin content; dw: Dry weight; TAA: Total antioxidant activity; DPPH: 2,2-diphenyl-1-picrylhydrazyl free radical scavenging activity (DPPH); FFD: Fractional factorial designs; CCRD: Central composite rotatable designs; TE: Trolox equivalent; CCD: Central composite design.
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MDPI and ACS Style

Seyyedi-Mansour, S.; Donn, P.; Carpena, M.; Chamorro, F.; Barciela, P.; Perez-Vazquez, A.; Jorge, A.O.S.; Prieto, M.A. Utilization of Ultrasonic-Assisted Extraction for Bioactive Compounds from Floral Sources. Biol. Life Sci. Forum 2024, 40, 15. https://doi.org/10.3390/blsf2024040015

AMA Style

Seyyedi-Mansour S, Donn P, Carpena M, Chamorro F, Barciela P, Perez-Vazquez A, Jorge AOS, Prieto MA. Utilization of Ultrasonic-Assisted Extraction for Bioactive Compounds from Floral Sources. Biology and Life Sciences Forum. 2024; 40(1):15. https://doi.org/10.3390/blsf2024040015

Chicago/Turabian Style

Seyyedi-Mansour, Sepidar, Pauline Donn, Maria Carpena, Franklin Chamorro, Paula Barciela, Ana Perez-Vazquez, Ana Olivia S. Jorge, and Miguel A. Prieto. 2024. "Utilization of Ultrasonic-Assisted Extraction for Bioactive Compounds from Floral Sources" Biology and Life Sciences Forum 40, no. 1: 15. https://doi.org/10.3390/blsf2024040015

APA Style

Seyyedi-Mansour, S., Donn, P., Carpena, M., Chamorro, F., Barciela, P., Perez-Vazquez, A., Jorge, A. O. S., & Prieto, M. A. (2024). Utilization of Ultrasonic-Assisted Extraction for Bioactive Compounds from Floral Sources. Biology and Life Sciences Forum, 40(1), 15. https://doi.org/10.3390/blsf2024040015

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