Ci a ion: Duque-So o, C.;
Ruiz-Va gas, A.; Rueda-Robles, A.;
Qui an es-Piné, R.; Bo ás-Lina es, I.;
Lozano-Sánchez, J. Bioac i e Po en ial
o Aqueous Phenolic Ex ac s o Spices
o Thei Use in he Food Indus y—A
Sys ema ic Re iew. Foods 2023,12,
3031. h ps://doi.o g/10.3390/
oods12163031
Academic Edi o : Hong Wu
Recei ed: 20 July 2023
Re ised: 8 Augus 2023
Accep ed: 10 Augus 2023
Published: 12 Augus 2023
Copy igh : © 2023 by he au ho s.
Licensee MDPI, Basel, Swi ze land.
This a icle is an open access a icle
dis ibu ed unde he e ms and
condi ions o he C ea i e Commons
A ibu ion (CC BY) license (h ps://
c ea i ecommons.o g/licenses/by/
4.0/).
oods
Re iew
Bioac i e Po en ial o Aqueous Phenolic Ex ac s o Spices o
Thei Use in he Food Indus y—A Sys ema ic Re iew
Ca men Duque-So o 1, Ana Ruiz-Va gas 1, Ascensión Rueda-Robles 1, Rosa Qui an es-Piné2,
Isabel Bo ás-Lina es 3,* and Jesús Lozano-Sánchez 1
1Depa men o Food Science and Nu i ion, Uni e si y o G anada, Campus Uni e si a io s/n,
18071 G anada, Spain; ca menduque@ug .es (C.D.-S.); [email p o ec ed].es (A.R.-V.);
ueda obles@ug .es (A.R.-R.); jesusls@ug .es (J.L.-S.)
2
Resea ch and De elopmen Func ional Food Cen e (CIDAF), Heal h Science Technological Pa k, A enida del
Conocimien o 37, Edi icio BioRegión, 18016 G anada, Spain; [email p o ec ed]
3Depa men o Analy ical Chemis y, Facul y o Sciences, Uni e si y o G anada, 18071 G anada, Spain
*Co espondence: ibo as@ug .es
Abs ac :
The in e es on he use o na u al sou ces in he ood indus y has p omo ed he s udy o
plan s’ phenolic compounds as po en ial addi i es. Howe e , he li e a u e has been ocusing on
essen ial oils, wi h e y ew s udies published ega ding aqueous ex ac s, hei phenolic composi ion,
and bioac i i y. A sys ema ic e iew was conduc ed on di e en da abases ollowing PRISMA
guidelines o e alua e he ele ance o he phenolic con en o di e en a oma ic spices (o egano,
osema y, hyme, ginge , clo e, and peppe ), as ela ed o hei bioac i i y and po en ial applica ion as
ood addi i es. Al hough di e en ex ac ion me hods ha e been applied in he li e a u e, he use o
g een app oaches using e hanol and deep eu ec ic sol en s has inc eased, leading o he de elopmen
o p oduc s mo e ap o human consump ion. The s udied plan s p esen an in e es ing phenolic
p o ile, anging om phenolic acids o la onoids, es ablishing a co ela ion be ween hei phenolic
con en and bioac i i y. In his sense, esul s ha e p o en o be e y p omising, p esen ing hose
ex ac s as ha ing simila i no highe bioac i i y han syn he ic addi i es al eady in use, wi h
associa ed heal h conce ns. Ne e heless, he s udy o spices’ phenolic ex ac s is somehow limi ed
o
in i o
s udies. The e o e, esea ch in ood ma ices is needed o mo e unde s anding o ac o s
in e e ing wi h hei p ese a ion ac i i y.
Keywo ds:
phenolic compounds; plan ex ac s; medicinal and a oma ic plan s; an ioxidan ac i i y;
an imic obial ac i i y; g een ex ac ion
1. In oduc ion
The p oduc ion o millions o ons o esidues e e y yea as a esul o a mode n
li es yle and i s impac on he en i onmen has become a ising public wo y. In esponse,
socie y has ocused on he de elopmen o mo e sus ainable and heal hy app oaches. Thus,
he use o na u al ag o- ood by-p oduc s as sou ces in he indus y has been p omo ed as a
g ea al e na i e o cu en ly used aw ma e ials [
1
]. This has also anspi ed in o he ood
indus y, whe e consume s seem o inc easingly p e e mo e na u al addi i es as opposed
o hei syn he ic coun e pa s, in luenced by he ecen conce ns abou hei heal h sa e y.
Medicinal and a oma ic plan s (MAPs) ha e been his o ically used o adi ional
medicine and pose as an in e es ing sou ce o bioac i e compounds, wi h p o en an ioxi-
dan and an imic obial ac i i ies [
2
]. The e o e, hey can po en ially be used in he ood
indus y o he delay o p e en ion o ood quali y loss caused by mic obial g ow h and
undesi able chemical eac ions [3].
Some o he mos enowned MAPs a e spices, many o which ha e been ecognized
as sa e o human consump ion, such as o egano, pa sley, osema y, o hyme. They a e
mainly used in ood p epa a ions as la ou ings and as al e na i es o sal consump ion
Foods 2023,12, 3031. h ps://doi.o g/10.3390/ oods12163031 h ps://www.mdpi.com/jou nal/ oods
Foods 2023,12, 3031 2 o 23
o people wi h high blood p essu e [
4
]. Addi ionally, hei consump ion has been ela ed
o p o ec ion agains ca dio ascula diseases, neu odegene a ion, ype II diabe es, and
cance [5].
Spices ha e al eady been used as aw ma e ials o a a ie y o indus ies (including
cosme ic, pha macological, and ood indus ies) as la ou ings, ood colou ings, essen ial
oils, swee ene s, o e en o hei nu aceu ical ac i i ies, mainly due o hei phenolic
composi ion [
6
–
8
]. Along wi h he inc easing in e es o he consump ion o mo e na u al
and en i onmen ally iendly oods, spices a e gaining a new ound in e es o hei
inno a i e use as a sou ce o hese na u al bioac i e compounds [9].
Phenolic compounds a e plan seconda y me aboli es consis ing o an a oma ic ing
wi h one o mo e hyd oxyl g oups and can be syn hesized using he shikimic acid o
ace a e pa hway [
10
]. Mo e han 8000 phenolic compounds ha e been desc ibed in MAPs,
which a e commonly classi ied as phenolic acids, la onoids, s ilbenes, and lignans [
11
].
In his ega d, he mos popula cha ac e iza ion echnique has been high-pe o mance
liquid ch oma og aphy (HPLC), al hough he Folin–Ciocal eu me hod has also been used
o de e mine o al phenolic compounds.
I mus be conside ed ha bioac i e compounds can be lipophilic, such as essen-
ial oils, oleo esins, cu cuminoids, and ca o enoids ha a e ex ac ed using non-pola
sol en s, o hyd ophilic, such as many polyphenols ha a e ex ac ed using mo e pola
sol en s [
12
]. As well-known impo an sou ces o phenolic compounds and p o oundly
e iewed in he p e ious li e a u e, essen ial oils ha e been widely s udied as addi i es o
ood p ese a ion [
13
,
14
]. Howe e , he inhe en cha ac e is ics o essen ial oils cons ain
hei composi ion p ima ily o he leas pola polyphenols, which a e also p esen in ela-
i ely low concen a ions. This ci cums ance could po en ially limi hei p ac ical u ili y. In
con as , he use o aqueous-based ex ac s ich in mo e pola phenolic compounds, which
appea in highe concen a ions, is, he e o e, e y p omising.
Phenolic compounds a e known o hei an ioxidan and an imic obial ac i i y, which
ha e sus ained hei in e es in he ood indus y [
15
–
17
]. The bioac i i y o phenols is
an in e es ing opic o hei use as ood p ese a i es. I s po en ial mainly depends on
hei con en and dis ibu ion in he plan , which is a ec ed by ac o s p e ailing du ing
he cul i a ion o plan s, such as he wea he , ype o soil, ype o c op, and sun exposu e,
among o he s [
18
]. The addi ion o hese compounds o he packaging o an imic obial
p o ec ion has al eady been s udied in a ious o ms: (a) in special s uc u es con aining
hem, (b) ei he in hei ola ile o non- ola ile o m, as polyme s, (c) as polyme coa ing,
(d) bound h ough ionic o co alen bonds, o (e) in insically in he packaging. In a simila
way, o hei con ol o lipid and pigmen oxida ion, hey ha e been s udied in oods as
(a) an edible coa ing o (b) eed on i s su ace [
19
]. Wi h he in en ion o ex ac ing and
concen a ing hese compounds, implemen a ion o bo h con en ional and mo e ad anced
ex ac ion echniques ha e been s udied [18].
As a as we know, his is he i s e iew ega ding he compa ison o he ex ac ion
echniques a ailable and he e alua ion o he mos ecen me hods, ocused on a mo e
en i onmen ally iendly and sa e app oach o human consump ion, as well as a s udy
o hei phenolic con en as ela ed o hei bioac i i y and po en ial use, as essen ial
aspec s in o hei legal conside a ion as addi i es [
20
]. As p e iously s a ed, he s udy
o phenolic compounds om spices has been ocused on hei essen ial oils. Fo his
eason, e en hough hey p esen g ea po en ial as sou ces o mo e pola and abundan
compounds, aqueous phenolic ex ac s ha e no been conside ed un il ecen ly, as hei
phenolic cha ac e iza ion is a he sca ce. Also, he e is a di e need o e alua e he e ec
ha di e en ex ac ion me hods and condi ions could ha e on he chemical composi ion
o ex ac s and i s ele ance o i s po en ial syne gis ic bioac i i y. Addi ionally, p e ious
e idence o hei bioac i i y and sa e y o applica ion in ood p oduc s is needed in o de
o enable hei legal use in he indus y, as s a ed by cu en legisla ion and media ed by
o icial o ganiza ions, such as he Eu opean Food Sa e y Au ho i y (EFSA) and he Food
and D ug Adminis a ion (FDA) [20].
Foods 2023,12, 3031 3 o 23
The aim o his sys ema ic e iew is o e alua e he e idence ega ding he p ese a i e
ac i i y o phenolic compounds om MAPs ex ac s, such as o egano (
O iganum ulga e
,
O iganum glandulosum), osema y (Rosma inus o icinalis L.), hyme (Thymus zygis g a-
cilis, Thymus memb anaceus, Thymus longi lo us), ginge (Zingibe o icinale), clo e (Euge-
nia ca yophylla a), and peppe (Pipe nig um), which may p omo e hei use in he ood
indus y. This main objec i e can be di ided in o he ollowing sub-objec i es: (1) de e -
mining phenolic compounds con en in plan ex ac s; (2) analyzing an ioxidan ac i i y o
polyphenol- ich ex ac s; and (3) s udying an imic obial ac i i y o hose ex ac s.
2. Ma e ials and Me hods
2.1. Sea ch S a egy
Sys ema ic esea ch was conduc ed ollowing PRISMA guidelines. PubMed and Sco-
pus da abases we e sea ched o selec pape s, including he phenolic composi ion o
ex ac s and hei bioac i i y in
in i o
and ood-applied s udies. This e iew ocuses on
sys ema ic e iews, me a-analyses, and andomized con olled s udies published in he
yea s
2001–2022
. No language il e was applied. Exclusion c i e ia we e: (1) es ic ed
access a icles, (2) non- ela ion o he subjec o s udy, and (3) a icles ocused on spices’
essen ial oils.
In addi ion, he PICO p ocess was ollowed using he ollowing pa ame e s: (1) Popu-
la ion:
in i o
analysis; (2) In e en ion: an ioxidan and an imic obial ac i i y; (3) Compa -
ison: human ood; and (4) Ou come: a oma ic plan s’ use wi h he echnological unc ion
being possible, sus ainable, and inno a i e.
As o eligibili y c i e ia, a icles no ocused on he subjec o in e es we e excluded
om he analysis, including a icles e alua ing essen ial oils and hose ha did no include
he selec ed plan amilies. The s udy selec ion p ocess is shown in Figu e 1.
Foods 2023, 12, x FOR PEER REVIEW 3 o 23
o enable hei legal use in he indus y, as s a ed by cu en legisla ion and media ed by
official o ganiza ions, such as he Eu opean Food Sa e y Au ho i y (EFSA) and he Food
and D ug Adminis a ion (FDA) [20].
The aim o his sys ema ic e iew is o e alua e he e idence ega ding he p ese a-
i e ac i i y o phenolic compounds om MAPs ex ac s, such as o egano (O iganum ul-
ga e, O iganum glandulosum), osema y (Rosma inus officinalis L.), hyme (Thymus zygis g a-
cilis, Thymus memb anaceus, Thymus longi lo us), ginge (Zingibe officinale), clo e (Eugenia
ca yophylla a), and peppe (Pipe nig um), which may p omo e hei use in he ood indus-
y This main objec i e can be di ided in o he ollowing sub-objec i es: (1) de e mining
phenolic compounds con en in plan ex ac s; (2) analyzing an ioxidan ac i i y o poly-
phenol- ich ex ac s; and (3) s udying an imic obial ac i i y o hose ex ac s.
2. Ma e ials and Me hods
2.1. Sea ch S a egy
Sys ema ic esea ch was conduc ed ollowing PRISMA guidelines. PubMed and Sco-
pus da abases we e sea ched o selec pape s, including he phenolic composi ion o ex-
ac s and hei bioac i i y in in i o and ood-applied s udies. This e iew ocuses on
sys ema ic e iews, me a-analyses, and andomized con olled s udies published in he
yea s 2001–2022. No language il e was applied. Exclusion c i e ia we e: (1) es ic ed ac-
cess a icles, (2) non- ela ion o he subjec o s udy, and (3) a icles ocused on spices’
essen ial oils.
In addi ion, he PICO p ocess was ollowed using he ollowing pa ame e s: (1) Pop-
ula ion: in i o analysis; (2) In e en ion: an ioxidan and an imic obial ac i i y; (3) Com-
pa ison: human ood; and (4) Ou come: a oma ic plan s’ use wi h he echnological unc-
ion being possible, sus ainable, and inno a i e.
As o eligibili y c i e ia, a icles no ocused on he subjec o in e es we e excluded
om he analysis, including a icles e alua ing essen ial oils and hose ha did no include
he selec ed plan amilies. The s udy selec ion p ocess is shown in Figu e 1.
Figu e 1. PRISMA scheme wi h a icles included in he p esen sys ema ic e iew.
Figu e 1. PRISMA scheme wi h a icles included in he p esen sys ema ic e iew.
2.2. Sea ch Fo mulas and Keywo ds
The sea ch o mulas and keywo ds used in he p esen sys ema ic e iew ha e a ied
depending on he in e es a hand: (a) Fo phenolic compounds: (He bs OR Spices OR
Foods 2023,12, 3031 4 o 23
A oma ic plan s OR plan ex ac ) AND (Phenol compounds OR polyphenols OR bioac i e
compounds) AND (Ex ac ion me hods OR ex ac ion OR cha ac e iza ion me hods) AND
(g een ex ac ion OR al e na i e echnologies); (b) Fo an ioxidan ac i i y: (He bs OR
Spices OR A oma ic plan s OR plan ex ac ) AND (Phenol compounds OR polyphenols
OR bioac i e compounds) AND (An ioxidan s OR Na u al an ioxidan s) AND (O egano
OR O iganum OR Thyme OR Thymus se pyllum OR Thymus plan OR Rosema y OR Ginge
OR Clo e OR Peppe ); (c) Fo an imic obial ac i i y: (He bs OR Spices OR plan ex ac )
AND (Phenol compounds OR polyphenols OR bioac i e compounds) AND (An imic obial
OR An i i al) AND (Food-p ese a ion OR Food sa e y).
3. Resul s and Discussion
3.1. Main Phenolic Compounds Iden i ied in Medicinal and A oma ic Plan s
In his e iew, he mos p ominen phenolic cha ac e iza ion s udies and ex ac ion
echniques ha e been compiled. The selec ion o a speci ic me hod and ex ac ion echnique
has depended on he physico-chemical na u e o he compounds o be ex ac ed, i s cos ,
and secu i y. The ac o s ha in luence he ex ac ion e iciency a e he chemical na u e
o he ex ac ion sol en , he pa icle size o he plan ma e ials, he sol en –solid a io,
empe a u e, and ex ac ion ime. Addi ionally, ex ac s o age condi ions ha e in luenced
i s shel li e and bioac i i y [2].
Ex ac ion echniques applied in he li e a u e ha e been (a) con en ional echniques;
(b) p essu ized liquid ex ac ion, as supe c i ical luids (PLE), subc i ical luids (SFE), and
accele a ed sol en s; (c) mic owa e-assis ed ex ac ion (MAE); o (d) ul asound-assis ed
ex ac ion (UAE). Howe e , mic owa e- and ul asound-assis ed ex ac ion ha e been he
mos widely used echniques o bioac i e compounds. The la e allows he ex ac ion o
s onge la o s and hei p ese a ion o a longe ime [
21
]. In addi ion, i s non- he mal
na u e allows a lowe nega i e e ec on basic physical and chemical pa ame e s, such as
o al acid, o al soluble solid, colo , elec ical conduc i i y, iscosi y, and densi y [22].
Al hough a mul i ude o sol en s om glyce ol o choline chlo ide ha e been applied,
he highes pe o ming and, he e o e, mos used a e e hanol and me hanol. This has been
obse ed in Bellumo i e al. (2016), whe e he use o e hanol and ace one as ex ac ion
sol en s in ul asound-assis ed ex ac ion (UAE) and mic owa e-assis ed ex ac ion (MAE)
imp o ed he ex ac ion yield o phenolic compounds, ob aining be e esul s han when a
double e hanol mace a ion as solid–liquid ex ac ion p ocesses was applied [23].
The impo ance o he selec ed sol en can be u he obse ed in P oes os and Ko-
mai is (2006), whe e ul asonically assis ed ex ac ion using wa e as a sol en educed
he amoun s o phenolic compounds as compa ed o he con en ional me hod [
24
]. Di -
e en ex ac ion sol en s we e compa ed: 60% me hanol, 60% ace one, wa e , and e hyl
ace a e/wa e (60:30, / ), wi h me hanol being he bes op ion o ex ac ing phenolic
compounds om plan issues. These esul s we e in line wi h hose p e iously published
by Wang, P o an, and Helliwell (2004) [
25
]. In his s udy, e hanol, me hanol, ace one,
and ace oni ile, all a 30% in wa e ( / ), we e e alua ed o he ex ac ion o osma inic
and ca eic acids and compa ed wi h he ex ac ion using wa e as he selec ed sol en .
Ex ac ion was simila when using e hanol, me hanol, ace oni ile, o ace one. Howe e ,
osma inic acid con en was 20% lowe when compa ed wi h he ex ac ion using wa e
as a sol en . This has also been obse ed in Bellumo i e al. (2016), whe e a low ex ac-
ion o o al phenolic con en (TPC) was epo ed when wa e was used as a sol en [
23
].
Addi ionally, he e iciency o me hanol and e hanol as ex ac ion sol en s was con i med
in Š a c-Gaji´c e al. (2013), whe e 70% me hanol p o ided he highes yield o TPC wi h
MAE, while la onoids we e ex ac ed mo e e icien ly in he mic owa e ield using 70%
e hanol [
26
]. Howe e , an assessmen o di e en ex ac ion sol en s has been es ic ed o
speci ic s udies and, while i would be ideal o e alua e his e ec h ough he li e a u e,
di e ences in he expe imen al condi ions applied o each ex ac ion echnique and he
e alua ed spice be ween s udies do no allow o his compa ison o be ca ied ou .
Foods 2023,12, 3031 5 o 23
Also, he use o a combina ion o eme ging echnologies has p esen ed a g ea po-
en ial o highe ex ac ion han using hese indi idual echniques [
27
]. This has been
obse ed in Tzima e al. (2021) whe e Pulsed Elec ic Field was used as a p e- ea men
s ep o imp o ing he ob en ion o phenolic compounds using UAE [
28
]. This e ec was
explained h ough an inc ease in solubili y o phenolic compounds and acili a ed pe -
meabili y h ough plan cell walls, acili a ing enhanced eco e y o ul asound-ex ac ed
bioac i e compounds.
E en hough he a o emen ioned me hods p o ide good ex ac ion esul s, hei
adequacy o he implemen a ion in ood p oduc s mus be add essed. In his sense,
he de elopmen o he so-called g een me hods has aken in e es , no only as mo e
en i onmen ally iendly app oaches bu also as mo e sui able o hei la e pu pose.
Rega ding g een me hods o he ex ac ion o bioac i e compounds, one o he mos
popula is he use o deep eu ec ic sol en s (DES). In Ba bie i e al. (2020), combina ions
o glyce ol:choline chlo ide (1:2 /w) and wa e (10% w/w), lac ic acid:choline chlo ide
(1:3 /w) and wa e (10% w/w), 1,2-p opanediol:choline chlo ide (1:2 /w) and wa e
(10% w/w)
, and oxalic acid:choline chlo ide (1:1 /w) and wa e (10% w/w) we e used
and compa ed wi h e hanol as a sol en [
29
]. In his case, he combina ion o sol en s
showed a highe an ioxidan capaci y han he alcoholic ex ac , measu ed wi h he 2,2-
diphenyl-1-pic ilhyd azil oxide deple ion (DPPH) and e ic- educing an ioxidan capaci y
(FRAP) assays. In addi ion, e hanolic ex ac p esen ed he lowes s abilizing abili y o he
phenolic compounds p esen in he ex ac . O e all, hese p omising esul s p opose he
use o GRAS (gene ally ecognized as sa e by he FDA) sol en s as g ea al e na i es o
he ob en ion o enhanced ex ac s in he ood indus y.
Rega ding he plan ma e ial, phenolic compounds can be ex ac ed om mul iple
pa s o he a oma ic plan , such as lowe s, lea es, o seeds. Howe e , as phenolic con-
en seems o a y be ween di e en plan s uc u es, lowe ex ac s seem o gene ally
p esen he highes p esence o polyphenols [
30
]. Howe e , o he s uc u es ha e also been
used. In he analyzed s udies, osema y polyphenols we e ex ac ed om lea es [
29
,
31
]
and b anches [
32
]. O egano phenolic ex ac s we e mainly ob ained om lea es [
32
].
As o hyme, ex ac s we e ob ained ei he om he lea es [
31
,
33
,
34
] o he lea es and
b anches [
32
]. Rosema y ex ac s we e ob ained om he hizome a ea [
35
,
36
] and, in he
case o clo es, om lowe s [
33
]. The es o he s udies do no indica e he pa o he
a oma ic plan om which he ex ac s we e ob ained.
As o cha ac e iza ion me hods, he mos used among he li e a u e we e HPLC and
he Folin–Ciocal eu me hod [
23
,
26
,
30
,
33
,
36
–
48
]. The combina ion o he o me coupled
wi h he mass spec ome y has also been widely used as an analy ical cha ac e iza ion
me hod. Among HPLC, no mal phase (NP-HPLC), e e se phase (RP-HPLC), and hy-
d ophilic in e ac ion liquid ch oma og aphy (HILIC-HPLC) ha e also been used [49].
Th oughou di e en s udies, ega dless o he ex ac ion me hod, he phenolic p o ile
o spices seems o be compa able. Main phenolic compounds cha ac e ized in di e en
spices can be ound in Table 1.
The main phenolic compounds iden i ied in he di e en species o o egano we e
simila , al hough a ia ions in hei con en may be p esen . Some o he main phenolic
compounds iden i ied in his spice belonged o phenolic acids, such as osma inic acid,
ca eic acid, gallic acid, p-couma ic acid, chlo ogenic acid, and e ulic acid [
24
,
36
,
38
,
43
,
48
].
S uc u es o he mos ele an phenolic compounds ound in he spices a e p esen ed
in Figu e 2. The men ioned acids a e widely known o hei g ea an ioxidan ac i -
i y. The p esence o la onoids, such as apigenin, lu eolin and que ce in, should also be
no ed [24,38,48].

Foods 2023,12, 3031 6 o 23
Table 1. Phenolic compounds cha ac e ized in di e en spices.
Spice Ex ac Phenolic Compound Ex ac ion Technique Ex ac ion Condi ions Cha ac e iza ion Technique Re e ences
O egano
Glycosyla ed la onoids: kaemp e ol-O-glucu onide
and lu eolin-7-O glucu onide. MAE. 100% wa e , 42 ◦C and 2 min.
ex ac ion ime. Folin–Ciocal eu. [38]
Rosma inic, ca eic, chlo ogenic, e ulic, gallic,
p-couma ic, sy ingic and anillic acids. Dynamic sonica ion
assis ed e hanol ex ac ion. 60% e hanol ( / ) a oom empe a u e,
0.25 h. LC ×LC-MS. [48]
Ca eic and ca eic-O-hexoside, p o oca echic,
osma inic, 3-, 4- and 5-O-ca eoylquinic,
couma oylquinic, e ulic-O-hexoside, e ulic,
p-couma ic, homo anillic-O-hexoside, gallic acids,
sy ingic, p- and m-hyd oxybenzoic,
kaemp e ol-3-O-glucoside, kaemp e ol, and que ce in.
SPE. Hyd oalcoholic sol en . Folin–Ciocal eu, HPLC
LTQ-O bi ap mass
spec ome y. [43]
Gallic acid, ca eic acid, gen isic acid, p-couma ic acid,
annyl acid, e ulic acid, sy ingic acid, ca echin, u in,
que ce in, apigenin, na ingenin, and e iodic yol UAE. 60% me hanol, 60% ace one, wa e
and e hyl ace a e/wa e [60:30, / ].
RP-HPLC and Folin–Ciocal eu.
[24]
Rosema y
Ca nosoic acid and osma inic acid. SFE. 40 ◦C and 300 ba . GC-FID, TLC [32]
Rosma inic acid, ca eine, 7-me hyl osmanol, u in,
na ingin, and e ulic acid. UAE.
Glice ol:choline chlo ide (1: 2 /w) and
wa e (10% w/w), lac ic acid:choline
chlo ide (1:3 /w) and wa e (10% w/w),
1,2-p opanediol:choline chlo ide (1:2 /w)
and wa e (10% w/w): deep eu ec ic
sol en s compa ed o pu e e hanol.
Folin—Ciocal eu. [29]
Phenolic acids (gallic acid, osma inic acid, p-couma ic
acid), la onoids (que ce in 3-O-galac oside, kaemp e ol
3-O-glucu onide), and e penoids ( osmanol, ca nosol,
ca nosic acid).
UAE and CE. 100% wa e and 50:50 e hanol:wa e . Folin–Ciocal eu and T iple
TOF-LC-MS-MS. [37]
Fla onoids (ci sima i in, genkwanin), osma inic acid
and e penoids ( osmanol, ca nosol, ca nosic acid). UAE and MAE. UAE: 140 W
MAE: N220 ba , 100 ◦C. HPLC-DAD-MS-TOF. [23]
To al polyphenols, la onoids, an hocyanins,
monome ic and condensed an hocyanins. MAE. Me hanol: wa e (70:30, / ), 70 ◦C. Folin–Ciocal eu. [26]
Fla onoids (lu eolin, apigenin, diosme in, ci sima i in,
genkwanin) and e penoids ( osmanol, ca nosol,
ca nosic acid). SFE and PLE. SFE: 150 ba 6.6% e hanol and 400 ba
wi h CO
2
, 40
◦
C. PLE: e hanol 150
◦
C and
wa e 100 ◦C and 200 ◦C, 20 min. HPLC-DAD-MS. [45]
Ca eic and ca eic-O-hexoside, p o oca echic,
osma inic, 3-, 4- and 5-O-ca eoylquinic,
couma oylquinic, e ulic-O-hexoside, e ulic,
p-couma ic, homo anillic-O-hexoside, gallic acids,
sy ingic, p- and m-hyd oxybenzoic,
kaemp e ol-3-O-glucoside, kaemp e ol, and que ce in.
SPE. Hyd oalcoholic sol en . Folin–Ciocal eu.
HPLC + LTQ-O bi ap
mass spec ome y. [43]
Foods 2023,12, 3031 7 o 23
Table 1. Con .
Spice Ex ac Phenolic Compound Ex ac ion Technique Ex ac ion Condi ions Cha ac e iza ion Technique Re e ences
Thyme
De i a i es o hyd oxycinnamic acid: ca eic acid
hexoside, osma inic acid and de i a i es o sal ianolic
acid-A. Glycosyla ed la onoids:
lu eolin-7-O-glucu onide and kaemp e ol-O
glucu onide.
MAE. 150 ◦C, 50% e hanol and 9.5 min. Folin–Ciocal eu. [38]
Rosma enic acid, me hyl osma na e, ca eic acid,
cinnamic acid, chlo ogenic acid, quinic acid, and
la onoids such as e ulic acid, apigenin, lu eolin, and
que ce in.
Mace a ion. Me anol, e hanol, die hyl e he and
hexane, 72 h. Folin–Ciocal eu and HPLC. [34]
Ca eic and ca eic-O-hexoside, p o oca echic,
osma inic, 3-, 4- and 5-O-ca eoylquinic,
couma oylquinic, e ulic-O-hexoside, e ulic,
p-couma ic, homo anillic-O-hexoside, gallic acids,
sy ingic, p- and m-hyd oxybenzoic,
kaemp e ol-3-O-glucoside, kaemp e ol, and que ce in.
SPE. Hyd oalcoholic sol en . Folin–Ciocal eu.
HPLC + LTQ-O bi ap mass
spec ome y. [43]
p-couma inic acid, kaemp e ol, epigenin, e ulic acid,
lu eolin, osma inic acid, gallic acid, epigenin, eugenol,
que ce in. UAE and CE. Wa e 100% and 50:50 e hanol:wa e . Folin–Ciocal eu and T iple
TOF-LC-MS-MS. [37]
Ginge To al soluble solids, o al polyphenols, la onoids and
non- la onoids, o al ca o enoids, and i amin C. UAE. Wa e as sol en , 40–70 ◦C and 30 min Folin–Ciocal eu. [22]
Peppe
Capsaicinoids (no dihyd ocapsaicin, capsaicin,
dihyd ocapsaicin, homocapsaicin, and
homodihyd ocapsaicin). UAE. Me hanol as sol en , 50 ◦C and 10 min. HPLC- luo esncence. [44]
Pipe ine and pipe ine acid, anisic acid, me hyl anisa e,
shikimic acid, me hyl shikima e. Oxida i e o s eam dis illed.
Pipe ine ex ac ion: E hanol, 80 ◦C, 2 h.
Pipe ine acid ex ac ion: Pipe ine
dissol ed in KOH/e hanol a 1
/4( / ), a
8◦C, 15 h.
1H NMR,
13C NMR, FTIR, and HPLC. [50]
Clo e Tannins, phenolic compounds, e penoids, glycosides.
ca diac. TPC (mg/g): Kaempe o l 5.839, Ca echin 0.0184,
Gallic acid 0.0169. Mace a ion. 80% e hanol a a a io o 1:5 (w: ) 24 h. GC-MS and HPLC-DAD. [40]
DPPH: diphenyl pic il hyd azyl; HPLC: high-pe o mance liquid ch oma og aphy; MAE: mic owa e-assis ed ex ac ion; MS: mass spec ome y; SFE: supe c i ical luid ex ac ion; SPE:
solid-phase ex ac ion; TLC: hin-laye ch oma og aphy; TOF: ime-o - ligh mass spec ome y; UAE: ul asound-assis ed ex ac ion.
Foods 2023,12, 3031 8 o 23
Foods 2023, 12, x FOR PEER REVIEW 8 o 23
Figu e 2. Mos ele an phenolic compounds in diffe en spices.
Rosema y ex ac s we e he mos s udied in e ms o op imiza ion o he ex ac ion
p ocess and cha ac e iza ion o bioac i e componen s, which could be ela ed o hei in-
dus ial use. This is also obse ed o hyme and o egano, widely s udied in compa ison
o o he spices, such as clo es and ginge , om which no signi ican esul s ha e been
ound. The main phenolic compounds iden i ied in osema y we e ca nosoic acid and os-
ma inic acid. Ex ac s o his spice con ain la onoids, like ca echin, que ce in, u in, na -
ingin, and kaemp e ol, and phenolic acids, like chlo ogenic acid, p-hid oxibenzoic acid,
and p o oca echuic acid [23,32,33,42].
Thyme ex ac s p esen ed osma inic acid, caffeic acid, cinnamic acid, chlo ogenic
acid, and e ulic acid, among o he compounds [34,37,38,43]. The main la onoids con-
ained we e apigenin, lu eonin, and que ce in. Phenolic con en has been abundan ly
quan i ied using he Folin–Ciocal eu me hod, bu he e is no much in o ma ion abou he
quan i ica ion o indi idual phenolic compounds, as well as a lack in gene al cha ac e i-
za ion o his genus [38].
As o peppe , i s main phenolic compounds we e capsaicinoids, such as no dihy-
d ocapsaicin, capsaicin, dihyd ocapsaicin, homocapsaicin, and homodihyd ocapsaicin
[44,50]. These bioac i e compounds we e ex ac ed using ul asound using me hanol as
he ex ac an sol en and cha ac e ized using HPLC wi h luo escence de ec ion and
monoli hic columns o sepa a ion [44].
I is impo an o no e ha since s udies e alua ing diffe en sol en s ound no di -
e ences be ween e hanol and me hanol, e hanol should be p e e ably selec ed o ood
applica ions due o i s GRAS sol en s a us. Fo i s applica ion in he indus y, sui abili y
o hese ex ac s o human consump ion needs o be conside ed. All subs ances isola ed
in he conside ed ex ac s and mos sol en s used o hei ex ac ion in he conside ed
s udies a e GRAS subs ances and, hus, ini ially conside ed as innocuous, making hem a
good al e na i e o chemical addi i es no mally used in he ood indus y.
Figu e 2. Mos ele an phenolic compounds in di e en spices.
Rosema y ex ac s we e he mos s udied in e ms o op imiza ion o he ex ac ion
p ocess and cha ac e iza ion o bioac i e componen s, which could be ela ed o hei
indus ial use. This is also obse ed o hyme and o egano, widely s udied in compa ison
o o he spices, such as clo es and ginge , om which no signi ican esul s ha e been
ound. The main phenolic compounds iden i ied in osema y we e ca nosoic acid and
osma inic acid. Ex ac s o his spice con ain la onoids, like ca echin, que ce in, u in,
na ingin, and kaemp e ol, and phenolic acids, like chlo ogenic acid, p-hid oxibenzoic acid,
and p o oca echuic acid [23,32,33,42].
Thyme ex ac s p esen ed osma inic acid, ca eic acid, cinnamic acid, chlo ogenic acid,
and e ulic acid, among o he compounds [
34
,
37
,
38
,
43
]. The main la onoids con ained
we e apigenin, lu eonin, and que ce in. Phenolic con en has been abundan ly quan i ied
using he Folin–Ciocal eu me hod, bu he e is no much in o ma ion abou he quan i ica-
ion o indi idual phenolic compounds, as well as a lack in gene al cha ac e iza ion o his
genus [38].
As o peppe , i s main phenolic compounds we e capsaicinoids, such as no dihyd o-
capsaicin, capsaicin, dihyd ocapsaicin, homocapsaicin, and homodihyd ocapsaicin [
44
,
50
].
These bioac i e compounds we e ex ac ed using ul asound using me hanol as he ex ac-
an sol en and cha ac e ized using HPLC wi h luo escence de ec ion and monoli hic
columns o sepa a ion [44].
I is impo an o no e ha since s udies e alua ing di e en sol en s ound no di -
e ences be ween e hanol and me hanol, e hanol should be p e e ably selec ed o ood
applica ions due o i s GRAS sol en s a us. Fo i s applica ion in he indus y, sui abili y
o hese ex ac s o human consump ion needs o be conside ed. All subs ances isola ed
in he conside ed ex ac s and mos sol en s used o hei ex ac ion in he conside ed
s udies a e GRAS subs ances and, hus, ini ially conside ed as innocuous, making hem a
good al e na i e o chemical addi i es no mally used in he ood indus y.
3.2. An ioxidan Capaci y Analysis in Spices
3.2.1. Main An ioxidan Me hods Applied o A oma ic Plan s
An abundance o an ioxidan ac i i y assays has been applied on spices in he li e -
a u e. These me hods can be based on hyd ogen a om ans e , such as Oxygen Radical
Foods 2023,12, 3031 9 o 23
Abso bance Capaci y (ORAC) o To al Radical-T apping An ioxidan Pa ame e (TRAP);
elec on ans e , such as FRAP; o in a mix o bo h phenomena, such as deple ion o
2,2’-Azinobis-3-e hyl-benzo hiazoline-6-sul onic acid (ABTS) o DPPH. In o de o measu e
he an ioxidan ac i i y o ex ac s accu a ely, choosing an adequa e assay based on he
chemicals o in e es and, abo e all, he ood ma ix in which i will be included a e c i ical.
ABTS and DPPH assays seem o be he mos used adical sca enging assays o
spices [
30
,
36
,
38
,
41
,
43
,
51
,
52
]. This can be ela ed o he con enience and adequacy o hese
me hods o a a ie y o condi ions, as well as hei bene i s. DPPH s ands ou as a as ,
simple, and inexpensi e assay, wi h ew s eps and eagen s needed, as well as wi h a high
epea abili y. Some disad an ages may be he use o o ganic sol en s, hei sensi i i y o
pH, and colo in e e ence ha could cause unde es ima ion o esul s [53].
On he o he hand, ABTS can be applied o ei he lipophilic o hyd ophilic samples,
wi h high ep oducibili y, which makes i a highly e sa ile assay. This me hod may
also ha e some disad an ages, such as i s sensi i i y o ligh and empe a u e o lack o
s anda diza ion, which makes i di icul o compa e in in e labo a o y s udies [53].
E en hough ela i ely less is used, ORAC, TRAP, and FRAP ha e also been desc ibed
in he li e a u e. As o ORAC, i s ele ance o he s udy o biologically ele an ee
adicals as well as he use o a ious ee adical gene a o s can be in e es ing, bu esul s
canno be exp essed in weigh , hinde ing in e s udy compa isons. On ano he no e, TRAP
may be sui able o s udying ac i i y agains po en an ioxidan s (such as hyd oxyl and
pe oxyl adicals). Las ly, FRAP mus also be conside ed as an easy and inexpensi e assay,
al hough ins abili y o oxygen elec odes, he use o low pH, o he lack o de ec ion o
SH-g oup an ioxidan s may cause some disad an ages [53–55].
Howe e , a combina ion o a ew assays mus be ca ied ou o ha e a ealis ic assess-
men o he an ioxidan capaci y o a sample. Mo eo e , he di e ence in na u e be ween
some o he assays as well as he exp ession o he esul s based on di e en s anda ds can
hinde he compa ison o di e en esul s and s udies.
3.2.2. An ioxidan Ac i i y and Main Phenolic Compounds Iden i ied in A oma ic Plan s
As has been es ablished in he li e a u e, he an ioxidan ac i i y o medicinal and
a oma ic plan s shows g ea po en ial o hei use in he ood indus y, which is e idence
o hei accep ance as ood addi i es. In his sense, an ioxidan po en ial o medicinal and
a oma ic plan s has been s udied h ough hei phenolic composi ion, as main con ibu o s
o his ac i i y, as p esen ed in Tables 1and 2. Phenolic con en o ex ac s o mul iple
MAPs ob ained h ough di e en ex ac ion p ocedu es has been e alua ed, as is he case
o Lamiaceae plan s, such as o egano, osema y, and hyme. Addi ionally, se e al s udies
ha e conside ed hei applica ion on a a ie y o ood ma ices.
An ioxidan po en ial o o egano has been e alua ed in ex ac s and applied on di e -
en ood ma ices h ough ABTS and DPPH me hods [
36
,
38
,
43
]. As o ex ac ion condi ions
o phenolic eco e y, MAE appea s o be one o he main echniques. In Nabe e al. (2019),
MAE phenolic ex ac s om O. glandulosum showed good an ioxidan po en ial [
38
]. When
phenolic compounds we e ex ac ed wi h MAE, lowe concen a ions o e hanol esul ed
in g ea e eco e y o compounds and enhanced an ioxidan ac i i y. S udies on o he
species o o egano (O. ulga e) p esen ed simila consis en high-an ioxidan esul s [
36
,
43
].
Ne e heless, he main phenolic composi ion appea s o be simila h oughou he s udies,
hough o al con en may a y. Many o he iden i ied compounds belong o phenolic acids,
such as ca eic o osma inic (known o i s g ea an ioxidan capaci y) as well as la onoids,
such as que ce in, apigenin, and kaemphe ol, mainly in i s glycosyla ed o ms.
Foods 2023,12, 3031 16 o 23
as a na u al an imic obial. Wa e and e hanol as sol en s we e compa ed, showing ha a
osema y e hanolic ex ac exhibi ed an inhibi o y e ec agains ou pa hogenic bac e ia
s ains (Esche ichia coli, Salmonella en e i idis, Bacillus ce eus, and S aphylococcus au eus) while
he aqueous ex ac was only e ec i e agains h ee s ains (Esche ichia coli, Bacillus ce eus,
and S aphylococcus au eus). Howe e , he highes MIC alues (% w/ ) we e ob ained om
wa e -ob ained ex ac s [31].
In Çelik e al. (2021), he an imic obial ac i i y o hyme ex ac s was e alua ed
h ough MIC alues in Mulle –Hill on aga using he aga -well di usion me hod [
56
].
The assayed ex ac achie ed inhibi ion o Bacillus ce eus 702 Roma and Mycobac e ium
smegma is ATCC607. In Bouymajane e al. (2022), an imic obial assays we e ca ied ou
using he mic odilu ion me hod in yp one soy yeas o e alua e he minimal inhibi ion
concen a ion and minimal bac e icidal concen a ion (MIC and MBC) [
67
]. Thus, Thymus
zygis g acillis p esen ed an an imic obial e ec on Esche ichia coli, Pseudomonas ae uginosa,
Salmonella yphimu ium, Lis e ia monocy ogenes, En e ococcus aecalis, and S aphylococcus
au eus. Ano he hyme ex ac was e alua ed in Mascolo i e al. (2022), whe e ex ac s we e
able o inhibi he g ow h o Esche ichia coli, Salmonella yphimu ium, En e obac e cloacae,
S aphylococcus au eus, Bacillus ce eus, and Lis e ia monocy ogenes [68].
Ginge ex ac s ha e p o ed o inhibi he p oli e a ion o di e en bac e ia, ungi,
and i uses in he p e ious li e a u e. These e ec s could be mainly ela ed o he sup-
p ession o bac e ial bio ilm o ma ion, e gos e ol biosyn hesis, and i al adhesion and
in e naliza ion [
69
]. In Chang, Wang, Yeh, Shieh, and Chiang (2013), he an imic obial
capaci y o Zingibe o icinale Roscoe agains human espi a o y syncy ial i us (HRSV) was
s udied using ELISA, whe e ginge was able o dec ease he i us p oli e a ion in espi a-
o y mucosa cell lines [
71
]. In Zhong e al. (2021), he an imic obial capaci y o di e en
ac ions o e hanolic ex ac s we e e alua ed in compa ison o essen ial oils [
73
]. F ac ions
we e ob ained by a combina ion o di e en aqueous e hanolic ex ac s e apo a ed and
edissol ed in wa e -sa u a ed E OAc. The E OAc soluble ac ion o e hanolic ex ac s
p esen ed signi ican an ibac e ial ac i i y, while he insoluble ac ion was inac i e. Then,
he ex ac was ac iona ed ia silica gel column ch oma og aphy in o eigh pa s acco ding
o hei pola i ies o s udy hem sepa a ely ( ac ions M1–M8). M1-M4 ac ions showed
po en ial o supp ess he g ow h o B. sub ilis while M3 p esen ed he lowe MIC alue
(1
µ
g/mL), and M2 showed highe inhibi ion wi h a MIC alue o 8
µ
g/mL agains he
same bac e ia. F ac ions M5-M8 we e inac i e a a concen a ion o 128
µ
g/mL agains all
bac e ia es ed. Among he ou ac i e ac ions (M1–M4), M3 showed he highes e icacy
agains he es ed mic oo ganisms. This high an ibac e ial ac i i y could be ela ed o i s
g ea con en in bioac i e componen s.
Clo e ex ac s ha e also been s udied o hei an imic obial po en ial. In his ega d,
Mos a a e al. (2018) e alua ed di e en e hanolic plan ex ac s agains Bacillus ce eus,
S aphylococcus au eus, Esche ichia coli, Pseudomonas ae uginosa, and Salmonella yphi [
35
].
Among he ex ac s conside ed, clo e e hanolic ex ac , along wi h Punica g ana um, showed
he bes an imic obial ac i i y in ish-de i ed p oduc s. Addi ionally, hei an imic obial
p ope ies a e u he demons a ed in Rosa io e al. (2021), whe e clo e ex ac s showed
an
in i o
an imic obial e ec agains u ina y ac in ec ions (UTI) caused by P o eus
mi abilis and S aphylococcus epide midis [
40
]. This bioac i i y has been excep ional o hei
aqueous ex ac s. A he same concen a ion o eugenol, he clo e ex ac showed be e
an ioxidan and an imic obial capaci y han i s espec i e essen ial oil. This could be ela ed
o di e ences in phenolic con en , as essen ial oils end o p esen mo e apola molecules as
well as a lowe concen a ion.
O e all, i could be conside ed ha hei an imic obial ac i i y depends on he bioac-
i e compound concen a ion: when i is low, phenolic compounds inhibi mic obial
enzyme ac i i y, whe eas a high concen a ions, hey induce dena u a ion o p o eins. The
na u e o unc ional g oups p esen in hese compounds should also be conside ed, as i
a ies be ween di e en phenolics. Fo example, hyd oxyl g oups could cause he decay o
a p o on mo i e o ce, deple ion o an ATP pool, and consequen ly, cell dea h [74].

Foods 2023,12, 3031 17 o 23
As obse ed, his bioac i i y places he s udied ex ac s as po en ial addi i es o
ood p oduc s. Mo eo e , hese p ope ies could also be conside ed o hei use in ood
packaging. Once pa hogens adhe e o he ood su ace and o m bio ilms, hei emo al
is di icul . The e o e, he de elopmen o an imic obial packaging, using ex ac s, could
imp o e ood quali y and sa e y, hus he use o hese ex ac s has g ea po en ial in he
ood indus y. Fo his eason, and in ela ion o new lines o esea ch, he manu ac u e o
an ibac e ial ood packaging, whe e plan ex ac s a e isola ed o combined wi h pho o-
dynamic inac i a ion (PDI), can be p o i able and sus ainable, as discussed in Olszewska,
G˛edas, and Simões (2020) [75].
3.4. S uc u e–Bioac i i y Rela ionship
An ioxidan ac i i y o phenolic compounds has been ela ed o i s s uc u e. I s
obse ed biological ac i i y has been associa ed wi h he compounds phenolic –OH g oup,
hyd ophobic p ope ies associa ed wi h he benzene ing, he me hyl and isop opyl g oups,
he binding a ini y o he guanine esidue o DNA, and he an i-in lamma o y, apop o ic,
and dis up i e ac i i ies on he cell memb ane [
76
]. Addi ionally, he p esence o a second
hyd oxyl o an amino g oup in o- o p-posi ion a e ela ed o a be e an i adical and
an ioxidan pe o mance [
77
]. The numbe and posi ion o hese hyd oxyl g oups and hei
in luence on bioac i i y has been es ablished in he li e a u e, as ela ed o hei s ong
dona ing e ec and o ma ion o a s able quinone [
78
,
79
]. In his scena io, an ioxidan
ac i i y could depend on in e ac ions be ween phenolic compounds and bac e ial cells’
su aces, un ela ed o a speci ic phenolic g oup.
In he s udied ex ac s, he o ho posi ion (ca echol g oups) among he a oma ic
phenolic ing seems o be he p edominan con igu a ion o mos o he phenolic acids
and o he phenolic compounds iden i ied. The p esence o hese mul iple –OH g oups is
p ominen in compounds, such as osma inic acid o lu eolin, u in, na ingenin, ca echin,
and hei de i a i es.
Rosma inic acid p esen s in i s s uc u e wo o ho-dihyd oxy g oups (ca echol s uc-
u e), which could be ela ed o i s high an ioxidan ac i i y. This compound has been
ound in mos s udied spices, showing high concen a ions especially in hose belonging
o he Lamiaceae amily. O egano and osema y also p esen high le els o ca eic acid
and o he ca eoyl de i a i es. Ha ing a highly simila s uc u e o osma inic acid, hei
p esence is ela ed o a highe sca enging ac i i y in he wo Lamiaceae spices. Ca eic acid
has also been ound in ginge ex ac s [80].
Phenolic di e penes, such as ca nosol and ca nosic acid, also p esen a ca echol s uc-
u e in hei a oma ic ing. Consequen ly, hei p esence in ce ain ex ac s can po en ially
impac hei a ibu ed an ioxidan ac i i y. F om o he spices belonging o he Lamiaceae
amily, osema y shows he highes concen a ions o hese phenolic compounds.
Fla onoids a e also ound in he men ioned ex ac s. In his case, hei an ioxidan
ac i i y esul s om he loca ion and p esence o hyd oxyl and oxo g oups and double
bonds [
81
,
82
]. Specially, some combina ions ha e been ela ed o highe biological ac i i y.
The p esence o a 4-oxo g oup wi h ei he an unsa u a ed bond be ween C2 and C3 o OH
g oups nea C3 and C5 has co ela ed wi h be e bioac i i y [83]. This has been obse ed
in some molecules ound in hese ex ac s, such as apigenin, que ce in, lu eolin, and u in.
Addi ionally, compounds, like lu eolin, also p esen a ca echol g oup in he B- ing, which
could enhance hei bioac i i y [83].
The men ioned la onoids ha e been iden i ied in osema y, hyme, o egano, and
clo e. Howe e , he a ia ion in he concen a ion o la onoids and o he compounds
(like p o oca echuic and chlo ogenic acid) in di e en s udies (which could be ela ed o
he ex ac ion condi ions and o he ac o s p e iously discussed) could lead o a educed
con ibu ion o he s udied ac i i y.
E en hough he conside ed Lamiaceae ex ac s appea o ha e a simila p o ile, ose-
ma y seems o exhibi highe an ioxidan ac i i y h oughou di e en s udies. This di -
e ence could be ela ed o he highe concen a ion o impo an an ioxidan molecules
Foods 2023,12, 3031 18 o 23
in i s ex ac s, as men ioned o osma inic acid, o he syne gis ic e ec o i s speci ic
polyphenolic combina ion as compa ed o o egano o hyme.
As o he an ioxidan ac i i y in clo e ex ac s, his has been ela ed o hei composi-
ion o gallic acid, la onols, and hyd olysable annins. The high concen a ion o gallic
acid speci ically and i s de i a i es, which p esen h ee hyd oxy g oups in hei s uc u e,
could be ela ed o hei high an ioxidan ac i i y, epo ed as he highes in compa ison o
o he 26 spices [36].
3.5. Compa ison o Spice Ex ac s wi h O he Common Addi i es
As hese ex ac s seem o ha e an ou s anding an ioxidan po en ial, i is in e es ing o
conside i s compa a i e s udy wi h addi i es al eady in use, bo h na u al and syn he ic,
o i s e alua ion o use in he ood indus y. Also, analyzing spices in ood ma ices o e s
impo an in o ma ion abou po en ial ac o s ha could in e e e in he inal p oduc s.
Me hanolic hyme ex ac s ha e al eady shown g ea e an ioxidan ac i i y han
known addi i es BHA, TBHQ, and
α
- ocophe ol [
34
]. As o ex ac ion sol en s, he bes
polyphenolic ex ac ion om hyme has been achie ed using lowe concen a ions o
e hanol wi h MAE [
38
]. In Bouymajane e al. (2022), an ioxidan capaci y o ex ac s om
ae eal pa s o Thymus zygis subsp. g acillis was e alua ed using DPPH, es ablishing an
IC50 o 0.234 ±0.001 mg/mL, highe han he e e ence s anda d BHT [67].
In Jaya hilakan, Sha ma, Radhak ishna, and Bawa (2007), he an ioxidan ac i i y o
clo e (Eugenia ca yophylla a) was e alua ed in mea , bo h cooked and chilled, and compa ed
wi h he an ioxidan s TBHQ and BHA [
62
]. Resul s showed ha an ioxidan ac i i y
p esen ed he ollowing o de : clo e ( inely pul e ized) > asco bic acid > cinnamon ( inely
pul e ized) and TBHQ > BHA. In he p esen s udy, as in he majo i y whe e he an ioxidan
and an imic obial capaci y o spices in ood a e compa ed, senso y cha ac e is ics, such as
mea colo and la o , a e also e alua ed, wi h he aim o analyzing he accep ance o he
inal p oduc wi h na u al addi i es by consume s. F esh a oma ic plan s a e mo e popula ,
bu d y ex ac s con ibu e mo e o he biological alue [30].
Addi ionally, he an imic obial capaci y o clo e ex ac s has been e alua ed in com-
pa ison wi h he addi i e TBHQ and e hanol [
46
]. MIC alues (
µ
g/mL) o G am-posi i e
and -nega i e bac e ia, espec i ely, we e 50 and 100 o an e hanolic clo e ex ac , 25 and
50 o TBHQ, and 50 and 100 o e hanol. A ela ion be ween a highe amoun o o al
phenolic compounds and a ela i ely high an ibac e ial ac i i y was obse ed. I was also
concluded ha he ex ac ion o bioac i e chemicals wi h high pola i y sol en s was mo e
e ec i e han ex ac ion wi h low pola i y sol en s.
Rega ding clo e, eugenol is i s main bioac i e compound, ound in concen a ions
anging be ween 9381 mg and 14,650 mg pe 100 g o esh plan ma e ial [
84
]. Com-
pa ed wi h BHT, clo es (sp ou s) we e he spice wi h he highes an ioxidan ac i i y
(168.660 mmol o T olox/100 g d y weigh ) and polyphenol con en (14.380 gallic acid
equi alen s/100 g d y weigh ) [
36
]. Simila esul s ha e been obse ed on cooked bee
pa ies, whe e clo e ex ac s p esen ed an inc eased an ioxidan po en ial on p o ein and
lipid oxida ion when compa ed wi h BHT and asco bic acid [63].
The an ioxidan capaci y o osema y ex ac included in po k pa ies was e alua ed
using i amin E as a con ol [
60
]. This was u he con i med by Seb anek e al. (2005),
whe e he an ioxidan e ec o osema y ex ac s on ozen aw sausages also p o ed o be
highe han BHA and BHT [
61
]. Resul s showed ha he ex ac s e a ded lipid oxida ion
du ing mea p ocessing. Also, in Zahid e al. (2020), asco bic acid was used o e alua e
he an ioxidan capaci y o clo es in cooked bee pa ies using he TBARS me hod [
63
]. I
was also concluded ha he addi ion o clo e as a na u al an ioxidan could educe he
oxida ion o p o eins and lipids and imp o e he o ganolep ic quali y o he ood p oduc .
Na u al compounds used as addi i es in ood could be a iable al e na i e o add ess
he p oblem o mic obial esis ance, cons i u e new sou ces o an ioxidan compounds,
and hampe he nega i e e ec s o some syn he ic compounds. Also, plan ex ac s ha e
he added alue o mee ing he equi emen s o ood sa e y because spices a e GRAS
Foods 2023,12, 3031 19 o 23
subs ances and do no ha e a nega i e impac on nu i ional and senso y a ibu es o
oods u s, p o iding ha he app op ia e con en should be aken in o accoun o his
pu pose [
82
]. Howe e , he e is s ill a lack o knowledge ega ding hei inclusion on
di e en ood ma ices and he e alua ion o bo h hei an imic obial and an ioxidan
ac i i ies on hese o mula ions. In his sense, s udies should also ake in o conside a ion
he implica ions o he in oduc ion o phenolic ex ac on ood colo , la o , odo , bi e ness,
and as ingency, and i s impac on consume accep ance should be e alua ed. Addi ionally,
i is necessa y o add ess he s abili y o hese bioac i e compounds in o mula ions du ing
ood s o age ime ha could p esen a limi a ion on hei applicabili y.
4. Conclusions
In he p esen sys ema ic e iew, he li e a u e ega ding medicinal and a oma ic
plan s’ ex ac s has been e alua ed. An abundance o ex ac ion echniques has been
applied h ough he li e a u e o he ob en ion o ela ed ex ac s. In his sense, he
de elopmen o p o ocols o en i onmen ally iendly echniques is an a ea o s udy o
in e es o he u u e o he ood indus y. These ex ac s p esen an in e es ing bioac i e
compound con en . While his has been e alua ed o some ex ac s, a lack o indi idual
and de ailed cha ac e iza ion o polyphenols has been ound in some s udies, which may
ha e hinde ed he s udy o he po en ial co ela ion o a speci ic phenolic composi ion wi h
hei obse ed an ioxidan capaci y.
Ne e heless, a high bioac i i y associa ed wi h hei phenolic con en has been ob-
se ed o he conside ed spices. While he e is a clea associa ion be ween phenolic
compounds and an ioxidan capaci y, his same echnological unc ion is no a ibu ed
o a single isola ed phenolic compound, bu o se e al oge he , which ac in syne gy. On
he o he hand, ela ionships be ween phenolic con en in ood and an imic obial capaci y
is no ye clea , al hough a highe amoun o hose compounds may be ela ed o highe
ac i i y. The e ec o spices on ood pa hogens depends on he phenolic con en , bu also
on he in e ac ion wi h o he ood componen s.
Spices’ ex ac s hus p esen g ea po en ial o hei use in he ood indus y. When
ans e ing he use o plan ex ac s as an ioxidan and an imic obial ma e ial in he ood
indus y, we ha e o ake in o accoun wo impo an aspec s: (1) I has o be conside ed ha
phenolic compounds included in ood could con ibu e o he colo , la o , odo , bi e ness,
and as ingency, so i is impo an o s udy and con ol he dose o plan ex ac s added o
ood; and (2) ca e ul conside a ions should be gi en o he s abili y o bioac i e compounds
du ing ood s o age ime. In his ega d, spices could be an a ac i e al e na i e no
only o imp o ing ood p ese a ion, bu also o help dec ease hei senso y e ec in
ce ain oods.
Au ho Con ibu ions:
Concep ualiza ion, J.L.-S. and I.B.-L.; me hodology, C.D.-S. and A.R.-V.;
in es iga ion, C.D.-S., A.R.-V., A.R.-R., R.Q.-P., I.B.-L. and J.L.-S.; w i ing—o iginal d a p epa a ion,
C.D.-S., A.R.-R. and A.R.-R.; w i ing— e iew and edi ing, R.Q.-P., I.B.-L. and J.L.-S.; supe ision,
J.L.-S. and I.B.-L. All au ho s ha e ead and ag eed o he published e sion o he manusc ip .
Funding: This esea ch ecei ed no ex e nal unding.
Da a A ailabili y S a emen :
No new da a we e c ea ed o analyzed in his s udy. Da a sha ing is
no applicable o his a icle.
Acknowledgmen s:
C.D.-S. is g a e ul o he Doc o al P og am in Nu i ion and Food Sciences,
Uni e si y o G anada (g an om he Regional Go e nmen o Andalucía PREDOC_00110).
Con lic s o In e es : The au ho s decla e no con lic o in e es .
Foods 2023,12, 3031 20 o 23
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