Ultrasound technology for the extraction of biologically active molecules from plant, animal and marine sources

Journal Pre-proof Ultrasound Technology For The Extraction Of Biologically Active Molecules From Plant, Animal And Marine Sources Shikha Ojha, Ramón Aznar, Colm O’Donnell, Brijesh K. Tiwari PII:

S0165-9936(19)30128-1

DOI:

https://doi.org/10.1016/j.trac.2019.115663

Reference:

TRAC 115663

To appear in:

Trends in Analytical Chemistry

Received Date: 11 March 2019 Revised Date:

23 August 2019

Accepted Date: 10 September 2019

Please cite this article as: S. Ojha, R. Aznar, C. O’Donnell, B.K Tiwari, Ultrasound Technology For The Extraction Of Biologically Active Molecules From Plant, Animal And Marine Sources, Trends in Analytical Chemistry, https://doi.org/10.1016/j.trac.2019.115663. This is a PDF file of an article that has undergone enhancements after acceptance, such as the addition of a cover page and metadata, and formatting for readability, but it is not yet the definitive version of record. This version will undergo additional copyediting, typesetting and review before it is published in its final form, but we are providing this version to give early visibility of the article. Please note that, during the production process, errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain. © 2019 Published by Elsevier B.V.

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ULTRASOUND TECHNOLOGY FOR THE EXTRACTION OF BIOLOGICALLY

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ACTIVE MOLECULES FROM PLANT, ANIMAL AND MARINE SOURCES

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Shikha Ojha1, Ramón Aznar1, Colm O’Donnell2 and Brijesh K Tiwari1

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Ashtown, Dublin D15KN3K, Ireland

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Department of Food Chemistry and Technology, Teagasc Food Research Centre,

School of Biosystems and Food Engineering, University College Dublin, Ireland

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Corresponding author:

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Brijesh K Tiwari

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Department of Food Chemistry and Technology, Teagasc Food Research Centre,

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Ashtown, Dublin, D15KN3K, Ireland

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Tel: +35318059785

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Email: [email protected]

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Abstract

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The extraction of target compounds from a range of matrices largely depends on

22

effectiveness and efficiency of the extraction technique(s) employed. The objective

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of this review is to discuss a range of ultrasound assisted extraction processes alone

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or in combination with other approaches. In recent years, ultrasound has proven to

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be effective in a range of applications for enhancing extraction yields with minimal or

26

no damage to the quality of extracted compounds. Ultrasound technology presented

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in this review highlights the application of ultrasound as a pre-treatment and for

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direct use in assisted extraction processes. The use of ultrasound for extraction

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applications from plant, animal, marine and food processing streams are

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comprehensively presented.

31 32

KEYWORDS

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UAE, by-products, polyphenols, pigments, fatty acids, polysaccharides, proteins

34

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1. Introduction

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Extraction is one of the most important unit operations for separation of target

37

molecules from a range of matrices for chemical analytics as well as for the

38

production

39

maceration, heat reflux and solid liquid extraction or Soxhlet have many reported

40

limitations including laborious, time consuming and energy intensive. Process

41

intensification using new technologies is imperative due to energy, economic and

42

environmental considerations and to maximize process efficiency. Emerging

43

extraction techniques have been proposed to overcome various reported

44

disadvantages associated with conventional extraction approaches [1]. A range of

45

techniques including the use of soundwaves [2], pulsed electric field [3], enzymatic

46

[4], microwave energy [5], super- and sub-critical fluid [6] have been proposed for a

47

range of biomass applications. The use of emerging extraction techniques alone or

48

in combination have been investigated for process intensification [2, 7, 8].

49

Application of emerging technologies for extraction can be employed for:

of

new

ingredients.

Traditional

extraction

techniques

including

50

•

Pre-treatment of biomass

51

•

Solid-liquid extraction (SLE) with appropriated solvent;

52

•

Solid-liquid separation by filtration or centrifugation;

53

•

Solvent removal and recycling under vacuum to eliminate every trace of

54 55

residual solvent in final extract. •

Refining or purification of crude extract

56 57

There are significant numbers of key review papers outlining the application of

58

emerging technologies for extraction of target biomolecules from a range of matrices.

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The focus of this review paper is to highlight the application of ultrasound technology

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for isolation of target molecules from a range of matrices. Various applications of

61

sound waves for recovery and challenges encountered in application of ultrasound

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are also outlined with advances in establishing mechanisms of actions are also

63

discussed.

64

2. Ultrasound technology

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Ultrasonic waves applied for improving extraction efficacy are mainly in a range of 20

66

– 1000 kHz. Ultrasonic waves are mechanical waves which are propagated through

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target matrices via compression and rarefaction. Propagation of these waves’

68

causes a negative pressure in the solvent and when a soundwave pressure of higher

69

intensities propagates through a solvent, formation of microscopically small voids or

70

bubbles occurs. When these voids or bubbles are filled with a gas or water vapour,

71

growth and shrinkage of bubbles occurs until they collapse resulting in the formation

72

of cavitation (Fig 1 (i-ii)). A majority of extraction of molecules applications are

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reported in the frequency range of 20 – 100 kHz where large cavitation bubbles are

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produced and collapse of these bubbles causes extreme mechanical shear forces.

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The size and radius of cavitating bubbles decreases with an increase in ultrasonic

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frequency and an increase in the ultrasonic power employed results in increase

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number of cavitating bubbles. These shear forces are capable of disrupting matrices

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via cavitation [9]. Ultrasound mechanisms of action resulting in enhanced extraction

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yields and disruption of matrices are discussed in detail elsewhere [2].

80

2.1. Ultrasound technology as a pre-treatment

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Pre-treatments can be defined as any process carried out in advance of an

82

extraction process, which aims to stabilize a material or facilitate an extraction step,

83

thus increasing the yield or the efficacy of a process [10]. Traditionally, biologically

84

active molecules have been obtained using solid-liquid extraction (maceration,

85

shaking, etc.), with prior pre-treatments (drying, grinding, etc.) carried out to

86

homogenize the sample and enhance the extraction process. Pre-treatments are one

87

of the most expensive and least mature technology steps involved in the process of

88

converting biomass into target compounds. Although many different types of pre-

89

treatments have been investigated in recent years, there is still a need to further

90

improve efficiency, reduce costs and develop more environmental friendly

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processes. Sound waves in a frequency range of 20 – 1000 kHz may be employed

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to generate varying levels of cavitation to cause disruption of matrices (Fig 1iii).

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Application of green extraction principles (energy consumption reduction, enhanced

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process efficiency and the use of environmentally safe solvents) [11] is desirable to

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achieve a satisfactory extraction of biologically active molecules. Ultrasound

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technology offers significant advantages when employed as a pre-treatment by (i)

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improving extraction yield by facilitating penetration of solvents, (ii) enhancing yields

98

with or without using solvents, suitable for generally recognized as safe (GRAS)

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solvents and (iii) enhancing extraction of heat-sensitive compounds with reduced

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thermal and oxidation of target compounds. In this regard, pre-treatment using

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sonication was found to be a useful step in enhancing the extraction yields of oils

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from almond, apricot, and rice bran, although non GRAS solvents were employed

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[12]. Recent trends in extraction techniques have largely focused on minimizing the

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use of toxic solvents through replacement by GRAS solvents or carrying out

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extractions processes without solvents where process optimization through use of

106

ultrasound technology plays an important role. When correctly applied and

107

optimized, US can help minimize the degradation of extractable components as it

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works at low extraction temperatures [13], and is suitable for extraction of biological

109

active compounds from a range of sources as helps to conserve their bioactive

110

properties and prevent loss of biological activity. High power ultrasound was

111

employed as a pre-treatment to investigate potential benefits to extract extra virgin

112

olive oil from olive paste. The results showed that ultrasound treatment significantly

113

(p < 0.05) increased oil yield extractability [14], in comparison with other studies

114

investigating oil extraction from several matrices [15, 16]. Also, ultrasound was

115

applied using water as a solvent water to simultaneously enhance protein and sugar

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release from soybeans [17]. A study carried out on germination of oats (Avena sativa

117

L.) showed that after pre-treatment with ultrasound there was a significant

118

enhancement of γ-aminobutyric acid, glutamic acid, alanine, free sugars, and

119

phenolic compounds production [18]. Romero-Díez and co-workers studied the use

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of US pretreatments to improve the extraction of anthocyanins from wine lees. They

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reported similar extraction yields were achieved for shorter extraction times using US

122

[19]. The authors explained that ultrasound enhanced the external mass transfer and

123

not the internal mass transfer, which was the limiting step for the pigment extraction.

124

However, in the same study, microwave pre-treatment increased the extraction yield

125

of the pigment. Microalgae are a good source of bioactive compounds (pigments,

126

proteins, polysaccharides, and long fatty acids), all of which have been widely used

127

in a range of industry sectors , including cosmetics, animal feed, human food

128

[20].Through the cell disruption ability of ultrasound owing to cavitation, the

129

extraction of lutein from chlorella (Chlorella pyrenoidosa) followed by subcritical fluid

130

extraction resulted in enhanced extraction yields of lutein compared to traditional

131

Soxhlet extraction [21]. Interestingly, ultrasound has also proved to be effective to

132

pre-treat samples during the drying step. Samples have reduced flavour loss and

133

can be stabilized at shorter drying times and hence are more suitable for heat-

134

sensitive compounds [22]. A recent study has reviewed this approach to dry fruits

135

and vegetables [23]. Table 1 list some examples of the uses of ultrasound as a pre-

136

treatment approach to improve extraction yields.

137

2.2. Ultrasound assisted extraction of molecules

138

The potential of ultrasound technology for clean and green extraction of molecules

139

from a range of matrices has been widely reported. Clean/green extraction has been

140

described by several researchers as a mass transport phenomenon where

141

components present in a matrix are transferred into a green solvent. Ultrasound

142

technology is a versatile low cost technology which requires minimal space, is less

143

sophisticated compared to other novel technologies and can be scaled up, provided

144

the intrinsic and extrinsic control parameters are optimised for the specific matrix

145

including solvent type, concentration, temperature, ultrasonic power and frequency,

146

to obtain the desired yields of target molecules. Selected examples of the use of

147

ultrasound assisted extraction processes are presented in Table 2.

148

2.2.1. Plant origin

149

The use of natural antioxidants in the food industry has increased in recent years

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and there is a growing interest in improving extraction processes using clean and

151

green solvents [24]. In this regard, ultrasound technology is reported to be an

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effective technique for extraction of biologically active molecules from plants. Recent

153

studies are summarized in Table 2.

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The extractions of oil rich in polyphenols using ultrasound from grape seeds was

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studied, reported advantages included lower solvent consumption and a short

157

extraction time, whereas similar oil/polyphenols yields were obtained [25], similar

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conclusions were reported for extraction of polyphenols from grapes [26]. A study

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carried out using perilla seeds (Perilla frutescens) and UAE after optimization of

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several parameters using response surface methodology, reported an enhanced

161

extraction of proteins [27], similar results were also reported for Ganxet beans

162

(Phaseolus vulgaris L. var. Ganxet) [28]. Although ultrasound is considered as a

163

non-thermal technology, the energy released to the system may increase

164

temperature above ambient temperature and can have a negative impact on the

165

extraction of proteins. Thus, temperature must be studied and controlled depending

166

on the target protein. Extraction of polysaccharides has also enhanced through the

167

application of ultrasound technology. Bioactive polysaccharide extraction from

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mulberry leaves using ultrasound technology gave higher yields and required a lower

169

water/raw material ratio [29], similar results were reported using fresh fruit

170

(blueberry, nectarine, raspberry, watermelon) and vegetables (garlic, Jerusalem

171

artichoke, leek, scallion, spring garlic and white onion) [30].

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Heating is the traditional method to extract phytochemicals from leaves, but it may

174

lead to degradation due to long extraction times required. An ultrasound assisted

175

extraction technique was employed to extract catechins from green tea leaves with

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an increased yield compared to traditional methods observed [31]. Vanillin extraction

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from vanilla pods was studied using ethanol and UAE, the extraction yield was

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similar to traditional extraction (Soxhlet) but required less time [32]. Also less energy

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and solvent were required for phytochemical extraction from jatropha and jojoba

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hulls using UAE compared to other methods [32]. After optimization of US to extract

181

anti-oxidants from rosemary, Paniwnyk and co-workers reported that UAE increases

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the extraction yields of carnosonic acid compared to traditional methods [33].

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Another study on the same herb and compound, showed that the extraction

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efficiency was significantly enhanced by UAE in aqueous extracts [33]. Da Porto and

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Decorti employed UAE with 70% ethanol for 5 min followed by vacuum distillation to

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extract flavour compounds from spearmint and compared the results with traditional

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steam distillation, highlighting that the UAE had advantages in terms of yield,

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selectivity, stability and quality of flavour compounds extracted [34]. Assami and co-

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workers Assami, Chemat, Meklati and Chemat [35] aromatizatized olive oil with carvi

190

seeds by direct immersion into olive oil followed by ultrasound application to the

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mixture to facilitate diffusion of carvone and limonene into the oil, reducing the

192

extraction time required from days with conventional maceration to 20 min. The

193

same approach was adopted to produce vegetable oil enriched with carotenoids [36].

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As can be seen in Fig 2, fewer processes are necessary compared to traditional

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solid liquid-extraction (SLE) with UAE, and with a bio-refinery approach carrot juice

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can be used for beverage applications and the carrot cake fraction can be used for

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animal feed.

198

2.2.2. Animal origin

199

Ultrasound has been studied in combination with alkaline hydrolysis to enhance liver

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protein extraction from chicken and also to improve surface hydrophobicity [37]. UAE

201

was employed to extract hemoglobin from animal blood with good results [38]. The

202

extraction of collagen from meat matrices was studied with and without US, and the

203

results showed that US was more suitable for difficult extractable residues [39]. An

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additional recent paper was published in this area [40].

205 206

2.2.3. Marine sources

207

Marine microalgae and macroalgae are a rich source of biologically active

208

compounds (proteins, fatty acids, polyphenols, etc.) that can be used in various food,

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nutraceutical, cosmetic, and pharmaceutical products (Table 2). The application of

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green analytical chemistry principles for extraction of bioactive compounds is of

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critical importance for environmentally friendly product development [41]. One of the

212

key challenges in releasing biocompounds from microalgae is to effectively disrupt

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their rigid, thick and complex cell wall [42]. Polyphenols extraction from

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Nannochloropsis spp. using different green solvents after UAE optimization, resulted

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in enhanced recovery yields [43]. After investigating two varieties of Chlorella, water

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was demonstrated to be the best solvent to extract proteins using the same

217

approach [42]. From the red macroalgae Porphyra yezoensis, taurine compound was

218

successfully extracted after optimizing the UAE process [44]. Fucose and uronic acid

219

were successfully extracted from Ascophyllum nodosum macroalgae using

220

ultrasound [45]. Laminarin extraction was also studied from A. nodosum and

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Laminaria hyperborean after UAE resulting in 5.82% and 6.24% yields on a dry

222

weight basis, respectively [46]. Another study showed that UAE was an effective

223

method for extraction and purification of phenolic compounds from Hormosira banksii

224

[47].

225

2.2.4 Food processing (by-product) streams

226

The use of a zero-waste approach to integrate food-waste valorization into a circular

227

economy approach is currently one of the hottest topics in sustainability research

228

[48]. More than 1,000 polyphenolic compounds generated from plants, fruits, and

229

vegetables wastes are used in beverages, bakery, and other food products, dietary

230

supplements, cosmetics, and feed [49]. The valorization and consequently reduction

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of food processing by-products (waste) can be achieved by the extraction of

232

biologically active molecules often discarded as waste such as fibres, proteins,

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polysaccharides, oils, and phytochemicals.

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UAE has been used to enhance recovery of valuable proteins from several food

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industry by-products [50]. The extraction yields of compounds from by-product

236

streams may increase by more than 20% using UAE compared to conventional

237

approaches [49]. As shown in Table 2, US treatment may increase the extraction of

238

bioactive compounds from apple pomace by more than 20% [51, 52]. Cocoa shells

239

were valorized to extract and characterize flavanols, methylxanthines, fatty acids,

240

fibers, yields around 15.8% w/w of cocoa butter were reported [48]. Goula et al. used

241

vegetable oils to extract carotenoids present in pomegranate peel using UAE [53].

242

Shellfish waste is a major environmental concern worldwide. Shellfish waste is a

243

potential source of many commercially valuable products, such as, chitin, calcium

244

carbonate, proteins, and carotenoids. Suryawanshi and co-workers recently

245

reviewed the use of UAE to extract biologically active compounds from shellfishery

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waste [54]. Ca. 40% of the total weight of mackerel is considered a by-product,

247

Alvarez et al. obtained satisfactory recovery of protein from such by-product using

248

UAE without affecting the amino acid profile [55].

249 250

3. Combination approach

251

The combination of ultrasound with other techniques either simultaneous or

252

sequential extraction process has shown significant advantages compared to

253

ultrasound treatment alone. Synergistic aspect of ultrasound with other techniques

254

including supercritical fluid carbon dioxide and pressurized liquid extraction has been

255

reported for improving extraction yields. The use of ultrasound as a tool to disrupt

256

target matrix and use of supercritical fluids or pressurized liquids for extraction has

257

shown promising approach. The application of ultrasound in combination with

258

microwave or enzymes is discussed in the following section.

259

3.1. Ultrasound and microwave

260

Recently, combined ultrasonic and microwave assisted extraction technology has

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attracted significant attention as an alternative approach to traditional extraction

262

methods. Figure 3 shows the schematic and commercially available combined

263

microwave and ultrasound assisted extraction system. The combination of

264

ultrasound and microwave radiations can provide various advantages including

265

improved extraction rate and reduced processing time. Microwave assisted

266

extraction (MAE) is an important technique for extracting valuable compounds from

267

different matrices. In MAE, the high extraction yield may be attributed to the

268

synergistic combination of two transport phenomena (heat and mass gradients)

269

working in the same direction [56]. As discussed in previous sections, there are

270

several advantages of using ultrasound in extraction including increased mass

271

transfer, cell disruption, improved penetration and capillary effects. Consequently,

272

combination of these technologies can enhance the extraction efficiency and may

273

result in several synergistic advantages including shorter extraction time, reduced

274

solvent requirements, improved energy efficiency and lower costs [57-59]. The

275

combination of microwave and ultrasound has been shown to have significant

276

advantages in extraction, production of biofuels, and production of oxide and metallic

277

nanopowders [60]. Ultrasonic-assisted extraction has been widely employed in the

278

extraction of various compounds including pectin. The first study to obtain phenolics

279

using simultaneous ultrasonic and microwave assisted extraction (UMAE) technique

280

was reported by Lou, Wang, Zhu, Zhang, Gao, Ma and Wang [61]. They reported a

281

significant reduction of extraction time and an improvement of efficiency with higher

282

phenolic yield compared to maceration. Chen, Gu, Huang, Li, Wang and Tang [62]

283

optimised ultrasonic/microwave assisted extraction (UMAE) conditions to maximize

284

the yield and purity of polysaccharides possessing anti-tumor activities from the

285

Inonotus obliquus fungus. Their results indicated that the UMAE had great potential

286

and efficiency compared with traditional hot water extraction with no significant

287

changes in anti-tumor activities. Alonso-Carrillo, de los Ángeles Aguilar-Santamaría,

288

Vernon-Carter, Jiménez-Alvarado, Cruz-Sosa and Román-Guerrero [63] carried out

289

extraction of phenolic compounds from Satureja macrostema using microwave-

290

ultrasound assisted and reflux methods. S. macrostema is an aromatic herb

291

containing polyphenolic compounds including flavonoids, which have been reported

292

to have antioxidant and hepatoprotective effects. Their results showed that

293

significant higher total phenolic content and lower median inhibition concentration

294

values compared to reflux extraction, resulting in a higher radical scavenging ability,

295

which can be attributed to the lower temperatures used in microwave-ultrasound

296

assisted extraction and the higher stability of the extracted compounds.

297 298

3.2. Ultrasound and enzyme assisted extraction

299

Enzyme assisted extraction has been shown to be effective in improving extraction

300

yields and is also considered as a gentle and environment-friendly extraction method

301

[64]. However, enzyme assisted extraction has some limitations including longer

302

extraction time and increased processing cost [65]. Enzyme assisted extraction

303

coupled with ultrasound irradiation has been reported to be an effective method for

304

extraction of target compounds with advantages of enhanced extraction yield,

305

reduced extraction time and physiological activities of the extracts [66]. Ultrasonic

306

and enzyme-combined extraction has shown to be suitable for use in juice extraction

307

[67, 68] and in extraction of bioactive compounds from various sources including

308

vegetables [69], fruits [66] and seaweed [70]. Wu, Zhu, Yang, Wang and Wang [69]

309

investigated ultrasonic-assisted enzymatic extraction (UAEE) to extract phenolics

310

from broccoli inflorescences in water rather than in organic solvents. A cocktail of

311

enzymes including cellulase, pectinase and papain coupled with a low-frequency

312

sonotrode (20 kHz) was investigated and optimised for maximum extraction yield with

313

significant free radical scavenging and total antioxidant activity. UAEE was used to

314

prepare Corbicula fluminea polysaccharide for potential superoxide radical

315

scavenging activity. UAEE extraction was employed for extraction of crude

316

polysaccharides from Trichosanthes Fructus (snake gourd fruit) which has significant

317

hypoglycemic, antioxidant and immunoenhancing activities [71]. Response surface

318

mythologies were applied to optimise the effects of pH, enzyme amount, extraction

319

temperature, and liquid-to-solid ratio on the extraction yields. Li, Mao, Wang, Raza,

320

Qiu and Xu [72] also applied UAEE to obtain the highest yield of phenolic content,

321

strongest antioxidant, and antitumor activities and to optimise the extraction

322

conditions of Trapa quadrispinosa Roxb. residues. UAEE has also been used for the

323

extraction of polysaccharide from animal sources. Liao, Zhong, Ye, Lu, Wang, Zhang,

324

Xu, Chen and Liu [73] employed UAEE for extraction of polysaccharides from Asian

325

clams (Corbicula fluminea), a freshwater bivalve mollusc. They observed a

326

significantly higher extraction yield of UAEE in 32 min compared to enzyme-assisted

327

extraction over 4 h. They also reported that the polysaccharide extracted by UAEE

328

had lower molecular weight, higher sulfate content and higher superoxide radical

329

scavenging activity compared to the polysaccharide extracted by enzyme extraction

330

alone.

331

332

4. Limitation of ultrasound assisted extraction

333

Ultrasound assisted process have several benefits over conventional extraction

334

either as a pre-treatment techniques followed by conventional technique or in

335

combination with other novel techniques. However, there are certain limitations

336

and challenges associated with the use of ultrasound at any stage of extraction

337

processes. One of the main limitations of ultrasound technology is related to the

338

scale-up challenges which are mainly due to non-uniform reporting of

339

processing conditions including actual power rather nominal power. This can be

340

overcome by employing standard methods for measurement and reporting of

341

ultrasonic power. Apart from scale-up challenges there are couple of technical

342

challenges which requires further developments these include reduction in wave

343

attenuation in high viscosity samples, decrease in ultrasonic wave with distance

344

cauing activated ultrasonic zone in close vicinity of the transducer and pitting of

345

ultrasonic transducers. Provided the standardised ultrasound extrinsic and

346

intrinsic process parameters are adopted, this will facilitate comparisons

347

between studies to evaluate the effects of ultrasound variables on extracted

348

bioactive yields.

349 350

4. Conclusions

351

Innovative technologies which can enhance processing efficiency, reduce energy

352

consumption, and produce high-quality ingredients with preserved biological activity

353

are required. The application of UAE as a clean, green and economic alternative to

354

conventional techniques has been widely investigated in recent decades. With the

355

recent advances in material science and development of robust, energy efficient

356

transducers, application of ultrasound at an industrial scale is increasingly being

357

employed. Along with a growing trend for environmentally friendly processes, the

358

food industry is interested in reducing production costs by either accelerating

359

processes or increasing yield. To encourage further industry adoption of ultrasound

360

technology to enhance process intensification in industrial large-scale extraction, it is

361

necessary to demonstrate US safety, sustainability, cost-effectiveness and eco-

362

friendliness

363

364

References

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[55] C. Álvarez, P. Lélu, S.A. Lynch, B.K. Tiwari, Optimised protein recovery from mackerel whole fish by using sequential acid/alkaline isoelectric solubilization precipitation (ISP) extraction assisted by ultrasound, LWT - Food Science and Technology, 88 (2018) 210-216. [56] F. Chemat, M. Abert-Vian, Y. Zill-e-Huma, Microwave assisted separations: green chemistry in action, Green chemistry research trends, Nova Science Publishers, New York, NY2009, pp. 33-62. [57] I.G. Moorthy, J.P. Maran, S. Ilakya, S. Anitha, S.P. Sabarima, B. Priya, Ultrasound assisted extraction of pectin from waste Artocarpus heterophyllus fruit peel, Ultrasonics sonochemistry, 34 (2017) 525-530. [58] K. Lefsih, D. Giacomazza, F. Dahmoune, M.R. Mangione, D. Bulone, P.L. San Biagio, R. Passantino, M.A. Costa, V. Guarrasi, K. Madani, Pectin from Opuntia ficus indica: Optimization of microwave-assisted extraction and preliminary characterization, Food chemistry, 221 (2017) 91-99. [59] S.-Y. Xu, J.-P. Liu, X. Huang, L.-P. Du, F.-L. Shi, R. Dong, X.-T. Huang, K. Zheng, Y. Liu, K.-L. Cheong, Ultrasonic-microwave assisted extraction, characterization and biological activity of pectin from jackfruit peel, LWT, 90 (2018) 577-582. [60] S. Dąbrowska, T. Chudoba, J. Wojnarowicz, W. Łojkowski, Current Trends in the Development of Microwave Reactors for the Synthesis of Nanomaterials in Laboratories and Industries: A Review, Crystals, 8 (2018) 379. [61] Z. Lou, H. Wang, S. Zhu, M. Zhang, Y. Gao, C. Ma, Z. Wang, Improved extraction and identification by ultra performance liquid chromatography tandem mass spectrometry of phenolic compounds in burdock leaves, Journal of Chromatography A, 1217 (2010) 2441-2446. [62] Y. Chen, X. Gu, S.-q. Huang, J. Li, X. Wang, J. Tang, Optimization of ultrasonic/microwave assisted extraction (UMAE) of polysaccharides from Inonotus obliquus and evaluation of its anti-tumor activities, International Journal of Biological Macromolecules, 46 (2010) 429-435. [63] N. Alonso-Carrillo, M. de los Ángeles Aguilar-Santamaría, E.J. Vernon-Carter, R. JiménezAlvarado, F. Cruz-Sosa, A. Román-Guerrero, Extraction of phenolic compounds from Satureja macrostema using microwave-ultrasound assisted and reflux methods and evaluation of their antioxidant activity and cytotoxicity, Industrial crops and products, 103 (2017) 213-221. [64] N.T. Huynh, G. Smagghe, G.B. Gonzales, J. Van Camp, K. Raes, Enzyme-assisted extraction enhancing the phenolic release from cauliflower (Brassica oleracea L. var. botrytis) outer leaves, Journal of agricultural and food chemistry, 62 (2014) 7468-7476. [65] H. Van Le, Comparison of enzyme-assisted and ultrasound-assisted extraction of vitamin C and phenolic compounds from acerola (Malpighia emarginata DC.) fruit, International journal of food science & technology, 47 (2012) 1206-1214. [66] W. Tchabo, Y. Ma, F.N. Engmann, H. Zhang, Ultrasound-assisted enzymatic extraction (UAEE) of phytochemical compounds from mulberry (Morus nigra) must and optimization study using response surface methodology, Industrial Crops and Products, 63 (2015) 214-225. [67] L.N. Lieu, Application of ultrasound in grape mash treatment in juice processing, Ultrasonics sonochemistry, 17 (2010) 273-279. [68] B. Dang, T. Huynh, V. Le, Simultaneous treatment of acerola mash by ultrasound and pectinase preparation in acerola juice processing: optimization of the pectinase concentration and pectolytic time by response surface methodology, DOI (2012). [69] H. Wu, J. Zhu, L. Yang, R. Wang, C. Wang, Ultrasonic-assisted enzymatic extraction of phenolics from broccoli (Brassica oleracea L. var. italica) inflorescences and evaluation of antioxidant activity in vitro, Food Science and Technology International, 21 (2015) 306-319. [70] D. Rodrigues, S.r. Sousa, A. Silva, M. Amorim, L. Pereira, T.A. Rocha-Santos, A.M. Gomes, A.C. Duarte, A.C. Freitas, Impact of enzyme-and ultrasound-assisted extraction methods on biological properties of red, brown, and green seaweeds from the central west coast of Portugal, Journal of agricultural and food chemistry, 63 (2015) 3177-3188. [71] F. Chen, D. Li, H. Shen, C. Wang, E. Li, H. Xing, L. Guo, Q. Zhao, J. Shi, H. Nguyen, Polysaccharides from Trichosanthes Fructus via ultrasound-assisted enzymatic extraction using response surface methodology, BioMed research international, 2017 (2017).

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575

Figures

576 577

Figure 1. (i) Cavitation bubble, (ii) in-situ formation and collapse of cavitation bubbles

578

in close vicinity of ultrasonic probe, (iii) SEM image of fresh meat surface (iiia) and

579

ultrasound treated meat surface (iiib) showing the disruption of matrices for

580

enhanced penetration of solvents, schematic of ultrasound probe based (iva) and

581

bath configuration (ivb).

582 583

Figure 2. Biorefinery approach for valorisation of carrots

584

585 586

Figure 3. Ultrasound in combination with microwave processor (a) commercially

587

available and (b) schematic diagram of ultrasound in combination with microwave

588

bath type system.

589

Table 1. Ultrasound technology as a pre-treatment approach to improve bioactive compounds extraction.

Matrix

Compounds

Technique

Solvent

Conditions

Result

Reference

Olives

Extra virgin

High power

No solvent

150 W and 20 kHz, 13.5 kJ kg−1

Increased extraction yield

[6]

olive oil

ultrasound (HPU)

used

(Sonics and Materials Inc., CT,

pre-treatment

USA), 6 minutes

followed by centrifugation partition Olives

Oil

Ultrasound-assisted

No solvent

Ultrasonic bath (Elmasonic S60H:

The main parameters to evaluate oil [7]

extraction

used

ultrasonic frequency—35 kHz;

quality were not affected by the US

effective ultrasonic power—150 W).

and the extraction yield as

10 min and 30 °C.

compared with the control when the oils were improved

Wine lees

Anthocyanins

UA pre-treatment

Ethanol and

BRASON (101-147-035) Sonifier®

anthocyanins extraction yield was

followed by SLE

Ethanol:water

Cell Disruptor Model 450. Time

not enhanced with the use of UA

varied (30 s and 90 s) and between 10 and 100% that correspond to an

[11]

amplitude value of the sound wave of 19 and 130 µm Water

Ultrasound (25 kHz) for 5 minutes

Ultrasound treatment significantly

Oats (Avena

Free sugars

The effects of power

sativa L.)

and phenolic

ultrasound on the

enhanced the free sugars and

compounds

nutritional properties

phenolic compounds in the

of germinated oats.

germinated oats after 96 h

Rapeseed

Oil Extraction

Ultrasound-assisted

Water

extraction plus SLE

Ultrasound bath (KQ5200DE, Kun

[10]

Good yields of oil extraction

[8]

124.01 crude extract when

[13]

Shan Ultrasonic Instruments Co., Ltd, China) for 1 min.

Chlorella

Lutein

UAE followed by

Water

Ultrasound bath

(Chlorella

subcritical fluid

compared with the Soxhlet

pyrenoidosa)

extraction

extraction 54.64 mg

Soy

Protein and sugars

UAE followed by SLE Water

Branson 2000 Series bench-scale

Disruption of the cell wall and

ultrasonic unit (Branson Ultrasonics

release of intracellular materials.

Corporation, Danbury, CT,

Improvements in protein (46%) and

USA), 2.2 kW, 20 kHz. 60 ºC, 30 min sugar (50%) release into water extracts 590

[9]

591

Table 2. Ultrasound-assisted extraction of biological active compounds from plants, animals, marine and by-products sources

Matrix

Compounds

Solvent

Conditions

Results

Reference

Rosmarinus

Carnosic acid

Ethanol

Comparison of several conditions: at 15 min, room

The maximum yield extraction was

[26]

temperature; (1) Conventional solvent extraction, (2) UAE

achieved with the probe.

officinalis L.

with a 40 kHz bath, (3) UAE with a 40 kHz bath and stirring, (4) UAE with a 20 kHz probe Rosmarinus

Carnosic acid

Water

A Hielscher ultrasonic processor UP400S (400 W, 24 kHz)

UAE using water or ethanol provides an

with a horn of 22 mm in diameter was used. Two test: a

extract of rosemary with equal or higher

discontinuous process, with 30 s ON/OFF cycles and a

antioxidant content as those produced

continuous process at 40 ºC for 7 min.

by other assisted extraction technique.

Ultrasonic sonifier (Sonoplus model HD 2200, Bandelin,

30 min UAE gave grape seed oil yield

(Vitis vinifera biocompounds

Berlin) equipped with a titanium alloy flat tip probe (13 mm

(14% w/w) similar to Soxhlet extraction

L.)

diameter) (TT13, Bandelin, Berlin) was used (20 KHz, 150

for 6 h and the fatty acid compositions

W).

was not affected significantly.

An ultrasonic system (REUS, France) 25 kHz

Faster transfer of biocompounds to the

officinalis L.

Grape seeds Oil and

Olive oil

Carvone,

-

-

limonene and

oil, enhancing quality and shelf life of

carotenoids

olive oil.

[16]

[17]

[28,29]

Perilla seeds Protein

Water

(Perilla

After oftimization, power of 61 W, extraction time of 12 min, Yield of the perilla meal proteins was and ratio of liquid to solid of 40 mL/g.

10.77%.

Ultrasound water bath at 40 kHz (Cole-Parmer 8890,

Ultrasound provided higher extraction

Vernon Hills, Illinois, USA) with constant shaking

efficiency and productivity. By studying

[19]

frutescens) Fruits and

Polysaccharids Ethanol

vegetables

[22]

the effect of various factors on the extraction (time, temperature, ethanol concentration) Mulberry

Polysaccharids Water

leaves

Tea leaves

Vanilla pods

Catechins

Vanillin

Water

Ethanol

Ultrasonic cleaner bath (Kunshan Ultrasound Instrument

The most promising technique was UAE [21]

Co., Ltd., Jiangsu, China) power of 60 W, 60 ºC, 20 min

in comparison with other techniques for

and ratio of water to raw material of 15:1

extracting polysaccharides

15 min using a Bandelin Ultrasonic Sonopuls GM 200

Sonication of green tea infusion

sonicator (Germany, microtips MS 72) with Water

enhances extraction of EGCG

Sonics vibra cell model (240 W, 22.4 kHz), operated in

Reduction of extraction time from 8 to 1

pulsed mode (5 s on followed by 5 s off) and operated at

hour

[23]

[24]

maximum supplied power. Mentha

Flavour

70%

Ultrasonic probe (Elettrofor Sonoplus model HD2200 with

Had advantages in term of yield,

spicata

compounds

Ethanol

TT13FZ probe, Bandelin, Berlin; 20 kHz, 200 W

selectivity, stability and quality of flavour

[27]

compounds extracted

Jatropha and Flavonoid,

Ethanol

No conditions of UAE were described

jojoba hulls

phenolic, and

with HCl

energy was developed to extract

saponin

or NaOH

flavonoid, phenolic, and saponin

compounds Mango

Carotenoids

A method using small solvent and

[25]

compounds from jojoba and jatropha Vegetable Ultrasonic 94 bath (Maxsell MX100QTD-3L at 100 W),

Other methods such us high shear

oil

dispersion techniques showed better

[30]

results than UAE Ganxet

Protein

beans

Alkaline

Ultrasonic bath (JP Selecta S.A., Barcelona, Spain)

US processing resulted in increased

solutions

operating at 4 ºC, 105 40 kHz, and 250 W for 30 or 60 min

yields, and percentages of material

(Phaseolus

[20]

solubilized and proteins recovered,

vulgaris L. var. Ganxet) Chicken liver Protein

Alkaline

Ultrasonic generator of 40°C 24 kHz and 300 W

water Chicken blood

Haemoglobin

Water

Better extraction results andimproved

[31]

the surface hydrophobicity S-4000 Ultrasonic Liquid Processor (Misonix, Farmingdale, Conclusion Ultrasonic processing is well [32] NY) 600 W and 20 kHz

suited to the application of blood cell

lysis because blood cells

Meat by-

Collagen

products

Water

ultrasonic processor (VCX 750; Sonics &

The use of UAE improves the efficiency

with

Materials,Newtown, CT, USA) 4 °C

extraction of natural collagen

[33]

pepsin Nannochloro Polyphenols

Water,

400S ultrasound equipment (Hielscher GmbH, Germany)

The extraction yields for UAE 2 times

psis spp.

ethanol,

400 W, 24 kHz, 30 min.

higher than that of conventional

dimethyl

[37]

extraction methods

sulfoxide Porphya

Taurine

Water

yezoensis

Ultrasonic device (20 kHz, 0–400 W; Type NP-B-400-15;

Rapid and efficient method was

Newpower Co. Ltd., Kunshan, China) pulse sequence was

established after optimization for the

20 s on and 5 s off

extraction and purification of taurine

[38]

from P. yezoensis Hormosira

Phenolic

Ethanol

banksii

compounds

70%

Ultrasonic bath (Soniclean, 220 V, 50 Hz and 250 W

Ultrasonic-assisted extraction using

[41]

RSM is effective for extraction and further isolation and purification of phenolic compounds

Ascophyllum Fucose and

Acid

VC 750, Sonics and Materials Inc., Newtown, USA) at a

This study demonstrates that ultrasound [39]

nodosum

uronic acid

water

constant frequency of 20 kHz, 750 W

assisted extraction (UAE) can be employed to enhance extraction of bioactive compounds from seaweed

Ascophyllum Laminarin

Acid

VC 750, Sonics and Materials Inc., Newtown, USA) at a

Ultrasound was demonstrated to be a

nodosum

water

constant frequency of 20 kHz, 750 W

more efficient method of extraction than

and

solid liquid extraction

Laminaria

based on laminarin content and

hyperborea

molecular weight distribution observed

[40]

in the extracts Chlorella

Protein

Methanol, Ultrasonicated at the frequency of 37 kHz for 1200 s

water appeared to be the preferable

sorokiniana

ethanol,

extractive solvent for use at the

and

1-

industrial scale with the advantages of

Chlorella

propanol,

low-cost, ubiquitous availability, minimal

vulgaris

2-

safety risks, and ease of upscaling

propanol and water

[36]

Cocoa shell

Flavanols,

waste

methylxanthine anol/hexa (150 W, 19.9 kHz) 40 °C

methylxanthines, fatty acids and fibres.

s, fatty acids

ne

Plus yields around 15.8% w/w of cocoa

and fibres

mixture

butter.

Polyphenols

Ethanol

Apple pomace Rice bran

Water/eth Titanium US horn (Danacamerini sas, Turin) for 15 min

PEX3 ultrasonic bath (25 kHz, 150 W)

50%

Rich source of flavanols,

[42]

Yield increased by more than 20% of the [45] extraction of bioactive compounds

Bioactive

Ethanol

Ultrasonic bath RK103H (BANDELIN SONOREX,

Ultrasonic technology was used for

extracts

67%

Germany) 54 °C, 45 min

extraction of the polyphenols and

[48]

antioxidants from rice bran using RSM Apple

Antioxidants

Water

pomace

Ultrasonic extraction reactor PEX1 (R.E.U.S., Contes,

Increase of more than 30% in total

France) 25 kHz, 150 W, 40 °C, 40 min

phenolic content when compared to

[46]

maceration Mackerelbyproduct

Protein

Water

Ultrasound processor (VC 750, Sonics and Materials, Inc.,

Ultrasound increased the amount of

(HCl 0.1

Newton, USA) 20 kHz, 750 W, 4 ⁰C, conducted for 10 min,

protein recovered using acid or alkali

M or

using a cycle of pulses of 5 seconds on and 5 seconds off,

extraction and amino acid profile was

NaOH 0.1 M)

not modified by extraction methods

[50]

Pomegranat e peels

Carotenoids

Vegetable VCX-130 (Danbury, CT, USA) sonicator equipped with a Ti- The green solvents extracted about 85.7 [47] oils

Al-V sonoprobe (13 mm) 130 W, 20 kHz 30 min. 51.5 °C

and 93.8% of the total carotenoids present in the waste material using UAE

592

HIGLIGHTS - Ultrasound technology can improve extraction yields - Ultrasound can be employed as a process or as a pre-treatments - Ultrasound assisted processes are suitable candidate for clean and green extraction - A range of biomolecules can be extracted using ultrasound