*Co esponding au ho : Tilo ma Sahu .
Copy igh © 2025 Au ho (s) e ain he copy igh o his a icle. This a icle is published unde he e ms o he C ea i e Commons A ibu ion Liscense 4.0.
Fo mula ion and e alua ion o sunsc een sp ay gel wi h lime peel ex ac (Ci us
au an i olia)
Mukesh Ba man and Tilo ma Sahu *
Rung a Ins i u e o Pha maceu ical Sciences, Bhilai, Du g, Cha isga h, India.
Wo ld Jou nal o Biology Pha macy and Heal h Sciences, 2025, 21(01), 224-234
Publica ion his o y: Recei ed on 25 No embe 2024; e ised on 04 Janua y 2025; accep ed on 06 Janua y 2025
A icle DOI: h ps://doi.o g/10.30574/wjbphs.2025.21.1.0005
Abs ac
Backg ound: P olonged exposu e o sunligh poses de imen al e ec s on he skin. Lime peel ex ac , con aining o e
60% la onoids, demons a es signi ican po en ial as a sunsc een agen due o he p esence o conjuga ed a oma ic
benzene ings capable o abso bing UV-A and UV-B adia ion. To mi iga e sun-induced skin damage, lime peel ex ac
has been o mula ed in o a sp ay gel, o e ing apid d ying p ope ies ha enhance use con enience and com o du ing
applica ion.
Objec i e: To e alua e he impac o a ying concen a ions o lime peel ex ac in sunsc een sp ay gel o mula ions on
hei physical p ope ies and in i o sun p o ec ion ac o (SPF) alues.
Me hods: Lime peel c ude ex ac was ob ained using 70% e hanol as he ex ac ion sol en . The ex ac was
inco po a ed in o sunsc een sp ay gel o mula ions a concen a ions o 5% (F1), 10% (F2), and 15% (F3). These
o mula ions we e assessed o hei physical p ope ies, including pH, iscosi y, sp eadabili y, d ying ime, and
adhesion, alongside hei in i o SPF alues.
Resul s: The concen a ion o lime peel ex ac signi ican ly in luenced bo h he physical p ope ies and SPF alues o
he sp ay gel o mula ions. All o mula ions (F1, F2, and F3) exhibi ed sa is ac o y physical s abili y and me he quali y
c i e ia o sp ay gel p epa a ions. The SPF alues o F1, F2, and F3 we e de e mined o be 15, 20, and 30, espec i ely,
indica ing a p og essi e inc ease in pho op o ec i e e icacy wi h highe ex ac concen a ions.
Conclusion: The sunsc een sp ay gel o mula ions con aining lime peel ex ac a concen a ions o 5% (F1), 10% (F2),
and 15% (F3) demons a ed physical s abili y and p o ided mode a e o high SPF p o ec ion. Among he o mula ions,
F3 (15%) exhibi ed he highes SPF alue o 30, sugges ing i s supe io e icacy as a sunsc een agen .
Keywo ds: Ci us au an i olia; Sp ay Gel; Topical Sunsc een Fo mula ion; Sp ay gel
1. In oduc ion
Ul a iole (UV) adia ion om sunligh , speci ically UV-A and UV-B ays, exe s dele e ious e ec s on he skin,
con ibu ing o p ema u e aging, sunbu n, and an inc eased isk o skin cance .¹ The human in egumen a y sys em
possesses inna e de ense mechanisms, including melanin syn hesis, s a um co neum hickening, and pe spi a ion,
which p o ide pa ial p o ec ion agains sola adia ion.² Howe e , hese na u al de enses a e o en insu icien ,
necessi a ing he use o exogenous pho op o ec i e agen s such as sunsc een o mula ions.³ Lime peel (Ci us
au an i olia) exhibi s po en ial as a na u al sunsc een agen due o i s high la onoid con en , exceeding 60%.⁴
Fla onoids, a p ominen class o seconda y me aboli es wi hin he phenolic compound g oup, possess s ong UV-
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225
abso bing p ope ies, e ec i ely mi iga ing UV-A and UV-B adia ion.⁵ The UV abso p ion po en ial o lime peel
la onoids has been co obo a ed by p elimina y s udies in ol ing o al phenolic con en assays.⁵ Resea ch has
demons a ed he e icacy o lime peel ex ac as a sunsc een ac oss a ious dosage o ms. Ex ac concen a ions ha e
yielded Sun P o ec ion Fac o (SPF) alues anging om 4.4 o 40.15,⁶ while gel, c eam, and lo ion o mula ions
inco po a ing he ex ac ha e achie ed SPF alues be ween 11.36–20.68, 12.01–18.57, and 11.27–19.44,
espec i ely.⁷,⁸ These indings subs an ia e he po en ial o lime peel ex ac as an e ec i e pho op o ec i e agen .To
u he ad ance he u iliza ion o lime peel ex ac in sunsc een o mula ions, his s udy ocuses on he de elopmen o
a sp ay gel, an inno a i e dosage o m o e ing apid d ying, enhanced use con enience, and imp o ed applica ion
consis ency. The objec i e is o e alua e he ex ac ’s impac on he physical cha ac e is ics, s abili y, and SPF alue o
he sp ay gel o mula ion, he eby es ablishing i s sui abili y as an e icien , use - iendly pho op o ec i e p oduc .
2. Ma e ials and me hods
2.1. Ma e ials
Lime (Ci us au an i olia), il e pape , dis illed wa e , absolu e e hanol, Folin-Ciocal eu eagen , aquabides, Ca bopol
940, HPMC, p opylene glycol, me hyl pa aben, p opyl pa aben, ie hanolamine, sodium ca bona e (Na₂CO₃), and gallic
acid we e ob ained om Sigma-Ald ich.
2.2. Equipmen
An o en (Memme ), g inde , dehyd a o , ho pla e (Philips), o a y e apo a o (Heidolph), wa e ba h (Memme ),
u nace, calipe s, analy ical balance (Me le Toledo), UV-Vis spec opho ome e (Shimadzu UV-1280), pH me e
(Me le Toledo), ul asonic cleane (B anson), iscome e (B ook ield LV), and magne ic s i e (C-MAG HS 7, IKA)
we e u ilized o he s udy.
2.3. Me hod
2.3.1. P epa a ion o simplisia
The lime samples we e ini ially au hen ica ed a he Bo anical Depa men o Science College, Du g, o con i m hei
iden i y as Ci us au an i olia. Ma u e lime ui s, cha ac e ized by hei da k g een colo , we e selec ed while s ill we
and ho oughly washed unde unning wa e o elimina e any di o impu i ies. The peels we e ca e ully sepa a ed
om he ui s using a lime peele . The collec ed peels we e d ied in a dehyd a o a 50 °C o one week o ensu e
comple e d ying. Once d ied, he he bal ma e ial was g ound in o a ine powde using a g inde .
2.3.2. Ex ac ion
The ex ac ion p ocess employed mace a ion wi h 70% e hanol. One kilog am o powde ed he bal ma e ial was soaked
in 10 li e s o 70% e hanol in a 1:10 (w/w) a io inside a co e ed con aine o 24 hou s, wi h s i ing o 10 minu es
each day. This mace a ion p ocess was epea ed h ee imes using 5 li e s o 70% e hanol in a 1:5 (w/w) a io. The
esul ing mace a e was il e ed h ough il e pape and e apo a ed using a o a y e apo a o a 75 mba p essu e and
a empe a u e o 50 °C. The liquid ex ac was u he concen a ed in a wa e ba h a 50 °C un il i eached a hick,
pas e-like consis ency9.
2.4. De e mina ion o o al phenolic con en
2.4.1. P epa a ion o gallic acid s ock solu ion
To p epa e a 1000 ppm gallic acid s ock solu ion, 10 mg o gallic acid was dissol ed in 10 mL o analy ical-g ade e hanol.
Se ial dilu ions o his s ock solu ion we e hen pe o med o achie e inal concen a ions o 5, 10, 20, 30, and 40 ppm.
2.4.2. P epa a ion o 7.5% Na2CO3 solu ion
A o al o 7,5 g ams o Na2CO3 we e weighed and dissol ed in 100 mL o dis illed wa e .10
2.4.3. De e mina ion o ope a ing ime (OT)
A 300 µL aliquo o a 30 ppm gallic acid solu ion was combined wi h 1.5 mL o Folin-Ciocal eu eagen , s i ed b ie ly,
and allowed o s and undis u bed o 3 minu es. Subsequen ly, 1.2 mL o a 7.5% Na₂CO₃ solu ion was added and mixed
ho oughly. The mix u e was hen le a oom empe a u e o he du a ion o he ope a ing ime. The abso bance o
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he solu ion was measu ed a 765 nm a in e als o e a 0–60 minu e pe iod, and he ime a which he abso bance
s abilized was eco ded as he ope a ing ime11.
2.4.4. De e mina ion o maximum wa eleng h
A 300 µL aliquo om each gallic acid solu ion (5, 10, 20, 30, and 40 ppm) was mixed wi h 1.5 mL o Folin-Ciocal eu
eagen . The mix u e was s i ed and allowed o s and o 3 minu es. Nex , 1.2 mL o a 7.5% Na₂CO₃ solu ion was added,
and he mix u e was ho oughly s i ed un il homogeneous. The solu ion was le a oom empe a u e o he ope a ing
ime (30 minu es). The abso bance was hen measu ed a he maximum wa eleng h o gallic acid, and a calib a ion
cu e was gene a ed based on he abso bance da a12.
2.4.5. De e mina ion o o al phenolic con en
The lime peel ex ac was p epa ed by dissol ing 10 mg o he ex ac in 10 mL o analy ical-g ade e hanol o achie e a
concen a ion o 1000 ppm. The ex ac solu ion was hen dilu ed wi h analy ical-g ade e hanol o a concen a ion o
100 ppm. Nex , 300 µL o he dilu ed ex ac solu ion was mixed wi h 1.5 mL o Folin-Ciocal eu eagen , shaken, and
allowed o s and o 3 minu es. A e wa d, 1.2 mL o a 7.5% Na₂CO₃ solu ion was added, and he mix u e was ho oughly
mixed and incuba ed o 30 minu es a oom empe a u e. The abso bance was measu ed a he maximum wa eleng h
o 745.8 nm. The phenolic con en was eco ded as he mg equi alen o gallic acid pe g am o sample. The
measu emen was epea ed h ee imes, and he o al phenolic con en was calcula ed using he ollowing o mula12:
To al Phenolic Con en =C x V x FP/g
No e: C = concen a ion (mg/mL; V = olume o ex ac (ml); FP = dilu ion ac o ; g = he weigh o sample used (g am)
2.4.6. Fo mula ion o sp ay gel p epa a ion
The o mula ion o he lime peel ex ac sp ay gel is ou lined in Table 1. Me hyl pa aben and p opyl pa aben we e
dissol ed in p opylene glycol. Ca bopol was dispe sed in ho dis illed wa e un il i became homogeneous, a e which
ie hanolamine was added, and he mix u e was homogenized wi h he me hyl pa aben solu ion. HPMC was g adually
added o a beake con aining ho dis illed wa e and s i ed un il ully dissol ed. The ca bopol mix u e was hen pou ed
in o he HPMC solu ion and sonica ed un il uni o m. The lime peel ex ac was dispe sed in dis illed wa e and sonica ed
o achie e a homogeneous ex ac solu ion. This ex ac was added o he HPMC and ca bopol mix u e, and dis illed
wa e was added o b ing he o al olume o 100 mL. The inal mix u e was sonica ed o 5 minu es be o e being illed
in o sp ay con aine s13.
Table 1 Fo mula o Sunsc een Sp ay Gel wi h Lime Peel Ex ac (Ci us au an i olia)
Ma e ials
Func ion o Ma e ials
Concen a ion o Ma e ials (%)
K-
F1
F2
F3
Lime peel ex ac
Ac i e ing edien
-
5
10
15
Ka bopol 940
Gelling agen
1
1
1
1
HPMC
Gelling agen
2
2
2
2
P opylene Glycol
Humec an
15
15
15
15
Me hyl pa aben
P ese a i e
0.18
0.18
0.18
0.18
P opyl pa aben
P ese a i e
0.02
0.02
0.02
0.02
T ie hanolamine
Alkalizing agen
qs
qs
qs
qs
Dis illed wa e ad
Sol en
100
100
100
100
*K- = Nega i e Con ol (wi hou addi ion o lime peel ex ac )
2.4.7. Tes ing o physical p ope ies o he p epa a ion
The physical p ope ies o lime peel (Ci us au an i olia) sp ay gel o mula ion we e es ed using he ollowing me hods
o each obse ed o mula wi h 3 eplica es14.
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pH Tes
The pH o he sp ay gel o mula ion was measu ed using a pH me e . The pH was assessed o ensu e i alls wi hin he
equi ed ange o opical applica ions (4.5–6.5), which helps p e en i i a ion15.
Viscosi y Tes
A 100 mL sample o he o mula ion was placed in a B ook ield iscome e wi h spindle numbe 61, se a a speed o 12
pm. The iscosi y eading was eco ded once he alue on he iscome e s abilized16.
Sp eadabili y Tes
The o mula ion was sp ayed on o a plas ic ilm om a dis ance o 5 cm, and i s sp eadabili y was assessed using a
calipe . The diame e o he sp ead a ea was measu ed as he pa ame e o e alua ion16.
D ying Time Tes
The o mula ion was sp ayed on o he inne o ea m o a olun ee om a dis ance o 5 cm. The ime aken o he
o mula ion o d y was eco ded using a s opwa ch17.
Adhesion Tes
Fo he adhesion es , he o mula ion was applied o he inne side o he lowe a m o a olun ee by sp aying i om
a dis ance o 5 cm. I he sp ay gel d ople s d ipped wi hin 10 seconds, i was a ed as "d ipping." I he d ople s
emained adhe ed o mo e han 10 seconds, i was a ed as "adhe ing."18
2.4.8. S abili y es ing o he p epa a ion
The p epa a ion was subjec ed o a cycle o cold s o age (4±2°C) o 24 hou s, ollowed by exposu e o a ho empe a u e
(40±2°C) o 24 hou s, cons i u ing one cycle. This p ocedu e was epea ed o a o al o 6 cycles. The physical changes
in he sp ay gel we e obse ed a he s a and end o each cycle, including assessmen s o o ganolep ic p ope ies, pH,
iscosi y, sp eadabili y, d ying ime, and adhesi e p ope ies.
2.4.9. SPF alue es ing o he p epa a ion
The de e mina ion o he SPF alue o lime peel ex ac begins wi h weighing each o mula ion, including F1 (5%), F2
(10%), F3 (15%), posi i e con ols (NIVEA® sunsc een sp ay SPF 30, Wa dah® UV Shield Essen ial Sunsc een Gel SPF
30, and Emina® Sun Ba le SPF 30), and nega i e con ol ( o mula ion wi hou ex ac ), amoun ing o 1 g am. The
co ec ion ac o (CF) is de e mined by measu ing he abso bance o he posi i e con ols, which ha e known SPF alues.
Each weigh ed o mula ion is combined wi h 50 mL o 70% e hanol and sonica ed o 15 minu es. The sonica ed
o mula ion is ans e ed o a 100 mL olume ic lask and illed wi h 70% e hanol up o he ma k. The o mula ion is
hen il e ed using il e pape , and he i s 10 mL o he il a e is disca ded. An aliquo ( il e ed o mula ion) o 100 μL
is pipe ed in o a 25 mL olume ic lask and dilu ed wi h 70% e hanol up o he ma k. Subsequen ly, he abso bance is
measu ed using a UV-Vis spec opho ome e . The abso bance spec um o he sample in solu ion o m is ob ained a
wa eleng hs anging om 290 o 320 nm wi h a 5 nm in e al, using 70% e hanol as he blank. The abso bance alues
o each concen a ion a e eco ded and used o calcula e he SPF alue .19 The SPF calcula ion acco ding o he Mansu
equa ion is as ollows, wi h EE x I ep esen ing a cons an ac o .
SPF = CF ×∑𝐸𝐸(ƛ) × 𝐼(ƛ) × 𝑎𝑏𝑠(ƛ)
320
290
No e: CF= Co ec ion Fac o ; EE= E y hema E ec ; I= In ensi y o sunligh ; abs = sample abso bance
3. Resul s and discussion
3.1. Ex ac ion
The ex ac ion in his s udy was pe o med using he mace a ion me hod, which is simple, does no in ol e hea ing, and
does no equi e special equipmen . The ma e ial was soaked o b eak he cell walls and memb anes h ough a p essu e
di e ence. Seconda y me aboli es in he cy oplasm a e dissol ed in he o ganic sol en (Di jen POM, 2000). The
ex ac ion o phenolic compounds was conduc ed using a mix u e o 70% e hanol and wa e . E hanol 70% has he
app op ia e pola i y o ex ac ing la onoids and annins. Addi ionally, i has low oxici y and eadily e apo a es.20
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S i ing was pe o med o achie e concen a ion equilib ium. The e-mace a ion p ocess was employed o ex ac any
emaining compounds in he esidue a e sol en sa u a ion.21 The il a e was concen a ed using a wa e ba h a 50°C,
esul ing in a concen a ed ex ac weighing 195.6 g ams wi h a yield o 19.55%. The yield alue is ela ed o he con en
o bioac i e compounds in he aw ma e ial. A highe yield co esponds o a highe desi ed subs ance con en (Di jen
POM, 2000).
3.2. De e mina ion o o al phenolic con en
The de e mina ion o o al phenolic con en was pe o med using he Folin-Ciocal eau eagen . Phenolic compounds can
eac wi h his eagen o o m a solu ion wi h measu able abso bance. The Folin-Ciocal eau eagen oxidizes he
hyd oxyl g oups o phenolic compounds, o ming a blue-colo ed complex. This eac ion p oceeds slowly unde acidic
condi ions, Na2CO3 was added du ing he es o c ea e a basic en i onmen and accele a e he eac ion.12
The s anda d solu ion used was gallic acid, which is a simple, na u al, and s able phenolic compound. Du ing he
eac ion, he hyd oxyl g oups in he phenolic compounds eac wi h he Folin-Ciocal eau eagen , o ming a blue-colo ed
molybdenum- ungs en complex. The in ensi y o he blue colo inc eases wi h he concen a ion o phenola e ions
o med. In o he wo ds, he highe he concen a ion o phenolic compounds, he mo e phenola e ions will educe he
he e opoly acid (phosphomolybda e-phospho ungs a e) o o m he molybdenum- ungs en complex, esul ing in a
da ke colo .12
The abso bance measu emen s o he gallic acid s anda d solu ion we e used o cons uc a calib a ion cu e. The cu e,
shown in Figu e 1, ollows a linea equa ion y = 0.0099x + 0.187 wi h a co ela ion coe icien (R) o 0.9989. This cu e
was used o de e mine he phenolic con en o he sample. The a e age o al phenolic con en o lime peel ex ac was
42.66 ± 0.25 mg GAE/g, indica ing ha each g am o lime peel ex ac is equi alen o 42.66 mg o la onoid.
Figu e 1 Gallic Acid S anda d Cu e
3.3. Tes ing o physical p ope ies o he p epa a ion
To achie e good and accep able pha maceu ical o mula ions in socie y, he physical p ope ies and s abili y o he
p epa a ions mus be examined. Physical p ope ies se e as de e minan s o he quali y o pha maceu ical
p epa a ions. The physical cha ac e iza ion es s include o ganolep ic e alua ion, pH, iscosi y, sp eadabili y, d ying
ime, and adhesion. The esul s o physical p ope y es s o he h ee o mulas can be obse ed in Tables 2 and 3.
Tabel 2 O ganolep ic es esul s o sunsc een sp ay gel o mula ion wi h lime peel ex ac
Fo mula
O ganolap ic
Fo m
Odo
Colo
Homogenei y
F1(5%)
Liquid
Lime smell
Yellow – b own
Homogeneous
F2(10%)
Liquid
Lime smell
B own
Homogeneous
F3(15%)
Liquid
Lime smell
Da k b own
Homogeneous
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Table 3 Resul s and signi icance es o sunsc een sp ay gel o mula ion wi h lime peel ex ac
Tes
Fo mula
Resul s ± SD
Requi emen
pH Tes
F1 (5%)
5.7 ± 0.03
4.5 – 6.5
F2 (10%)
5.5 ± 0.05
F3 (15%)
5.2 ± 0.05
Viscosi y
F1 (5%)
83.76 ± 0.97
< 150 cP
F2 (10%)
115.07 ± 1.40
F3 (15%)
139.28 ± 1.78
Sp eadibili y Tes
F1 (5%)
6.2 ± 0.03
5 -7 cm
F2 (10%)
5.6 ± 0.07
F3 (15%)
5.1 ± 0.07
D ying Time Tes
F1 (5%)
1.2 ± 0.08
< 5 minu es
F2 (10%)
2.4 ± 0.06
F3 (15%)
3.3 ± 0.11
Adhesion Tes
F1 (5%)
37± 1
> 10 seconds
F2 (10%)
62 ± 2
F3 (15%)
83 ± 2
3.4. O ganolep ic es
The h ee o mulas ha e he same colo and homogenei y, bu hey di e in consis ency and colo . A good o mula ion
is cha ac e ized by a pleasan odo , a ac i e colo , good consis ency, and homogenei y. The consis ency o he sp ay
gel p epa a ion is in liquid o m, in acco dance wi h i s de ini ion, which is one o m o gel o mula ion de elopmen ,
which is a wa e -based phase sys em comp ising a leas 10% o 90% o he o mula ion's weigh . The e m 'sp ay' is
de ined as a composi ion ha can be dispensed om i s applica o , such as an ae osol o sp ay pump. A homogeneous
o mula ion e e s o a p epa a ion ha does no con ain coa se pa icles, has e enly dispe sed pa icles, and has a
uni o m colo .22 Al hough he p epa a ion is in liquid o m, he consis ency o each o mula is di e en . Fo mula III (F3)
has he hickes consis ency because i has he highes concen a ion o lime peel ex ac , which is 15%. This esul
p o es ha he highe he concen a ion o he ex ac , he hicke he esul ing o mula ion, wi h a mo e in ense colo
pigmen a ion.
3.4.1. pH es
The ob ained esul s indica e ha an inc ease in he concen a ion o lime peel ex ac has an e ec on he pH alue o
he o mula ion, causing i o dec ease. This is due o he highe concen a ion o salicylic acid, amino acids, ci ic acid,
and i amin C in he lime peel ex ac . As a esul , he pH alue o he o mula ion dec eases. All o mula ions ha e me
he equi emen o a good pH alue, which is in line wi h he pH o he skin anges om 4.5 o 6.5. I he sp ay gel
o mula ion is oo acidic, i may cause skin i i a ion. On he o he hand, i he pH o he o mula ion is oo alkaline, i
may lead o d yness o he skin23.
3.4.2. Viscosi y es
The ob ained esul s indica e ha an inc ease in he concen a ion o lime peel ex ac a ec s he iscosi y alue o he
o mula ion, leading o an inc ease in iscosi y. This is because highe concen a ions o lime peel ex ac esul in a
hicke o mula ion. Viscosi y also in luences he sp eadibili y, d ying ime, and adhesion o he esul ing o mula ion
(Lachman e al., 2008). All o mula ions ha e me he equi emen o a good iscosi y alue o he sp ay gel
o mula ion, which is below 150 cP.24
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3.4.3. Sp eadibili y es
The esul s ob ained indica e ha as he concen a ion o lime peel ex ac inc eases, he sp eadibili y alue o he
o mula ion dec eases. This is because highe concen a ions o lime peel ex ac lead o a hicke o mula ion, educing
i s abili y o sp ead. Consequen ly, he oppo uni y o he ac i e ing edien s o come in o con ac wi h he skin
diminishes, esul ing in a dec ease in he e ec i eness o he o mula ion when applied opically.25 All o mula ions
demons a ed a sp eading pa e n when sp ayed and me he equi emen o an ideal sp eadibili y alue o he sp ay
gel o mula ion, which is 5-7cm.26
3.4.4. D ying ime es
The esul s ob ained indica e ha as he concen a ion o lime peel ex ac inc eases, he d ying ime o he o mula ion
also inc eases. This is because highe concen a ions o lime peel ex ac esul in a hicke o mula ion, which equi es
mo e ime o d y. All o mula ions ha e me he equi emen o a good d ying ime alue o he sp ay gel o mula ion,
which is less han 5 minu es o p e en s ickiness on he skin and p o ide com o o he consume when applied.10
3.4.5. Adhesion es
The esul s ob ained indica e ha as he concen a ion o lime peel ex ac inc eases, he adhesion alue o he
o mula ion also inc eases. This is because highe concen a ions o lime peel ex ac esul in a hicke o mula ion,
leading o a longe adhesion ime and inc eased elease o ac i e ing edien s. A sunsc een o mula ion is expec ed o
adhe e o he skin o a longe pe iod o ime o p o ide p olonged p o ec ion agains ul a iole adia ion.10 All
o mula ions can be conside ed o adhe e well o he skin as long as he o mula ion d ople s do no d ip om he skin
wi hin less han 10 seconds.27
3.5. S abili y es ing o he p epa a ion
The en i e sunsc een sp ay gel o mula is s o ed a a cold empe a u e o 4°C ± 2°C o 24 hou s and a a high
empe a u e o 40°C ± 2°C o 24 hou s (1 cycle). A e ha , a physical s abili y es is conduc ed o 6 cycles. The esul s
o he physical s abili y es o he sunsc een sp ay gel o mula ion can be seen in Tables 4 and 5.
Tabel 4 O ganolep ic s abili y es esul s o sunsc een sp ay gel o mula ion wi h lime peel ex ac
Fo mula
Cycle
O ganolep ic
Fo m
Odo
Colo
Honogenei y
F1(5%)
0
Liquid
Lime smell
Yellow – b own
Homogeneous
6
Liquid
Lime smell
Yellow – b own
Homogeneous
F2(10%)
0
Liquid
Lime smell
B own
Homogeneous
6
Liquid
Lime smell
B own
Homogeneous
F3 (15%)
0
Liquid
Lime smell
Da k b own
Homogeneous
6
Liquid
Lime smell
Da k b own
Homogeneous
Table 5 Resul s and signi icance o he physical s abili y es o he sunsc een sp ay gel o mula ion
Tes
Fo mula
Resul s ± SD
Requi emen
Cycle 0
Cycle 6
pH Tes
F1 (5%)
5.7 ± 0.03
5.6 ± 0.05
4.5 – 6.5
F2 (10%)
5.5 ± 0.05
5.4 ± 0.05
F3 (15%)
5.2 ± 0.05
4.9 ± 0.07
Viscosi y
F1 (5%)
83.76 ± 0.97
82.74 ± 1.51
< 150 cP
F2 (10%)
115.07 ± 1.40
112.07 ± 1.56
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F3 (15%)
139.28 ± 1.78
137.04 ± 1.71
Sp eadibili y Tes
F1 (5%)
6.2 ± 0.03
6.2 ± 0.03
5 -7 cm
F2 (10%)
5.6 ± 0.07
5.7 ± 0.08
F3 (15%)
5.1 ± 0.07
5.3 ± 0.05
D ying Time Tes
F1 (5%)
1.2 ± 0.08
1.1 ± 0.05
< 5 minu es
F2 (10%)
2.4 ± 0.06
2.2 ± 0.05
F3 (15%)
3.3 ± 0.11
3.2 ± 0.22
Adhesion Tes
F1 (5%)
37± 1
33 ± 2
> 10 seconds
F2 (10%)
62 ± 2
55 ± 2
F3 (15%)
83 ± 2
71 ± 2
3.5.1. O ganolep ic es
The o ganolep ic p ope ies obse ed in he o mula ion include he o m and consis ency, colo , odo , and
homogenei y o he sp ay gel. The esul s o he o ganolep ic es ing o sunsc een sp ay gel o mula ions F1, F2, and F3
indica e ha he e we e no changes in odo , colo , and o m o he o mula ion, and no isible phase sepa a ion
h oughou he 6 cycles o s o age, bo h a cold and high empe a u es. This indica es ha he sp ay gel o mula ion
exhibi s good s abili y in o ganolep ic es s o e he 6-cycle s o age pe iod.
3.5.2. pH es
The ob ained esul s indica e ha he o mula ion is s able, bu he e is a dec ease in pH du ing he s abili y es .
Changes in pH alues du ing s o age indica e eac ions o damage o he componen s wi hin he o mula ion, esul ing
in an inc ease o dec ease in pH alue.28 This can occu due o oxida ion eac ions on he ca boxylic acid g oups o he
acid compound in he ex ac , leading o he addi ion o hyd ogen a oms and a dec ease in pH alue. Addi ionally, he
use o anspa en packaging is ano he ac o con ibu ing o he ins abili y o he pH in he o mula ion as i allows
ligh o in e ac and cause deg ada ion eac ions o seconda y me aboli es in he o mula ion.29 This can be add essed
by s o ing he o mula ion in a place ha is no exposed o ligh and a an app op ia e empe a u e. The choice o
packaging should be ailo ed o he p ope ies o he ac i e subs ance and should p o ec he p oduc om ex e nal
in luences. The use o bu e s is also necessa y in he o mula o main ain he s abili y o he pH.
3.5.3. Viscosi y es
The ob ained esul s indica e ha he o mula ion is physically uns able in e ms o iscosi y, bu i s ill mee s he
iscosi y accep ance c i e ia o a sp ay gel. The dec ease in iscosi y can be a ibu ed o s o ing he o mula ion a
high empe a u es, which causes he ac i e molecules in he o mula ion o mo e, weakening he in e molecula
in e ac ions and esul ing in a dec ease in iscosi y .8 Choosing an ideal s o age empe a u e is impo an o main ain
he iscosi y s abili y o he o mula ion. S abili y es ing o he iscosi y o he sp ay gel is c ucial o ensu ing ha he
o mula ion emains easy o sp ay h ough he applica o and adhe es o he skin.
3.5.4. Sp eadibili y es
The ob ained esul s indica e ha he o mula ion is physically uns able in e ms o sp eading powe , bu i s ill mee s
he accep ance c i e ia o sp eading powe in a sp ay gel. This is due o a dec ease in iscosi y a e s o age, esul ing
in he weakening o he gel ma ix's s eng h in he o mula ion, which leads o an inc ease in he sp eading powe o
he o mula ion.30
3.5.5. 30D ying ime es
The ob ained esul s indica e ha he o mula ion is physically uns able in e ms o d ying ime, bu i s ill mee s he
accep ance c i e ia o d ying ime in a sp ay gel. This is due o a dec ease in iscosi y a e s o age, esul ing in he
o mula ion becoming mo e wa e y, which leads o a as e d ying ime.14
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3.5.6. Adhesion es
The ob ained esul s indica e ha he o mula ion is physically uns able in e ms o adhesion powe , bu i s ill mee s
he accep ance c i e ia o adhesion powe in a sp ay gel. This is due o a dec ease in iscosi y a e s o age, esul ing
in he o mula ion becoming mo e wa e y, which leads o a dec ease in he adhesion powe o he o mula ion.14
3.5.7. SPF alue es ing o he p epa a ion
The de e mina ion o he co ec ion ac o (CF) alue in his s udy was done by measu ing he abso bance o sunsc een
p oduc s wi h known SPF alues o ensu e he calcula ion o SPF based on he o mula. The abso bance alues we e
hen p ocessed using he Mansu equa ion o de e mine he CF alue used o accoun o he spec opho ome y and
sol en usage (Allen & Ansel, 2014). The posi i e con ol sunsc een p oduc s used in his s udy included NIVEA®
sunsc een sp ay SPF 30, Wa dah® UV Shield Essen ial Sunsc een Gel SPF 30, and Emina® Sun Ba le SPF 30. The esul s
o he Co ec ion Fac o (CF) o he Posi i e Con ol o he Sunsc een Fo mula ion can be seen in Table 6
Table 6 Resul s o co ec ion ac o (CF) o posi i e con ol o sunsc een o mula ion
Posi i e Con ol
SPF
Co ec ion Fac o (CF)
Resul s ± SD
NIVEA®
30
47.97
44.17 ± 0.05
Wa dah®
30
40.29
Emina®
30
44.25
Table 7 Resul s and signi icance o sp es ing o he sp ay gel
Fo mula
Resul s ± SD
SPF Ca ego ies
F1(5%)
15 ± 0.2
Medium
F2(10%)
20 ± 0.4
Medium
F3(15%)
30 ± 0.1
High
Figu e 2 G aph o a ia ion in ex ac concen a ion agains SPF alue
The selec ion o h ee di e en p oduc s wi h known SPF alues as posi i e con ols aimed o alida e he chosen
me hod o his s udy. The a e age CF alue ob ained om hese h ee p oduc s was 44.17. This CF alue would hen
be used o calcula e he SPF alue o he samples es ed in his s udy. The SPF alue es ing on he nega i e con ol
( o mula ion wi hou ex ac ) yielded an SPF alue o 1,8872. The SPF alue o he nega i e con ol indica ed ha he
polyme in he gel sp ay wi hou ex ac had no signi ican e ec on he SPF alue o he esul ing gel sp ay o mula ion.
The esul s o he SPF alue es ing o he gel sp ay o mula ion can be seen in Table 7, along wi h he g aph showing
he a ia ion o ex ac concen a ion on he SPF alue in Figu e 2.
In acco dance wi h he da a p esen ed in Table 7, he SPF alues de i ed om he h ee o mula ions a e classi ied
wi hin he medium o high ange. This classi ica ion is es ablished acco ding o he p o ec ion ange de ined by he
