Dinnimath et al Journal of Drug Delivery & Therapeutics.

2014; 4(6):68-74 68

Available online on 15.11.2014 at http://jddtonline.info

Journal of Drug Delivery and Therapeutics
Open access to Pharmaceutical and Medical research
© 2014, publisher and licensee JDDT, This is an Open Access article which permits unrestricted noncommercial use, provided the original
work is properly cited

RESEARCH ARTICLE

FORMULATION AND SPECTRAL ANALYSIS OF NEW POLY HERBAL TOOTHPASTE

S.Abhay 1, B M Dinnimath2* and K K Hullatti3
1
KLES College of Pharmacy Belgaum, India
2
Dept of Pharmaceutical Chemistry, KLES College of Pharmacy Belgaum, India
3
Department of Pharmacognosy, KLES College of Pharmacy Belgaum, India

ABSTRACT
Toothpaste is an agent used as an effective home care system. It is a paste or gel dentifrice used with a toothbrush as an
accessory to clean and maintain the aesthetics and health of teeth by the patients to enhance oral hygiene. What many people
don’t know is that most brand-name toothpaste contains a number of ingredients that are not healthy. Herbal toothpaste does
not contain the artificial colors, flavours or fluoride that many of the artificial products do contain. For the present study the
extracts of apple peel, lemon peel, orange peel, banana peel, clove oil were used to formulate a polyherbal toothpaste and
studied by phytochemical tests and spectral analysis using UV/VIS, IR spectroscopy. These studies have revealed the presence
of vital constituents which shall be responsible for anti-microbial activity and useful in tooth decay problems.
Keywords: Toothpaste, polyherbal toothpaste, antimicrobial activity

INTRODUCTION
Toothpaste is a common product in our families and people Most of the toothpastes contain sodium Lauryl Sulfate
hardly care to know about the product which ‘they are (SLS) which is an anionic compound in the toothpaste it can
using. Toothpaste is an agent used as an effective home care deactivate cationic agents present in the tooth paste.
system. It is a paste or gel dentifrice used with Abrasives constitute at least 50% of typical toothpaste.
a toothbrush as an accessory to clean and maintain the These insoluble particles help remove plaque from the teeth.
aesthetics and health of teeth by the patients to enhance oral They remove plaque and helps to minimize cavities and
hygiene. Toothpaste is used to promote oral hygiene. periodontal disease. Representative abrasives include
Although, brushing teeth twice a day and daily flossing is particles of aluminum hydroxide (Al(OH)3), calcium
highly effective in plaque reduction, over 50% of adults carbonate (CaCO3), various calcium hydrogen phosphates,
have gingivitis on an average of 3 to 4 teeth. Bacteria in various silicas and zeolites, and hydroxyapatite
dental plaque are one of the main factors causing (Ca5(PO4)3OH) (Perlich, et al., 1995) 3.
periodontal inflammation therefore, careful plaque control is
Fluoride in various forms is the most popular active
very important. However, mechanical plaque removal is
ingredient in toothpaste to prevent cavities. Fluoride occurs
inadequately performed by most members of the population.
in small amounts in plants, animals, and some natural water
The need for additional help in controlling bacterial plaque
sources. The additional fluoride in toothpaste has beneficial
provides the rationale for patients to use antimicrobial
effects on the formation of dental enamel and
dentifrices in addition to their mechanical oral hygiene
bones. Sodium fluoride (NaF) is the most common source
regimens.1
of fluoride, but stannous fluoride (SnF2), olaflur (an organic
What many people don’t know is that most of the salt of fluoride), and sodium
branded toothpastes contains a number of ingredients that monofluorophosphate (Na2PO3F) are also used. Stannous
are not healthy for the people or the environment. Bleach fluoride has been shown to be more effective than sodium
and peroxide are commonly used as whitening agents in fluoride in reducing the incidence of dental caries and
commercial toothpastes. But both bleach and peroxide can controlling gingivitis(Debjit b, et al., 2012) (George O et
be an irritant to the mouth and skin in small doses and are al., 1997 )(Kozisek F, 2004) (Diankov S, 2011) (Zia-ur-
considered to be hazardous materials because they can Rehman, 2006)4,5,6,7,8,9.
cause severe chemical burns in large doses. Artificial
flavorings and scents are commonly made from synthetic *Corresponding author
chemicals derived from petrochemicals or coal tar.. Mr. Basavaraj M Dinnimath,
Commercial toothpaste ingredients also affect the Dept of Pharmachemistry,
environment. EDTA (ethylenediaminetetraacetic acid) and KLEU’S College of Pharmacy,
formaldehyde are commonly used a preservatives in Belgaum, India-590010,
toothpaste and many other cosmetics and personal care Email: [email protected]
products. They are known environmental pollutants Phone: 919632045496, 8880124102
(Wolfgang W, 2005)2.

© 2011-14, JDDT. All Rights Reserved ISSN: 2250-1177 CODEN (USA): JDDTAO
Dinnimath et al Journal of Drug Delivery & Therapeutics. 2014; 4(6):68-74 69

India is a country which has medicines dating back to rotavapour. The excess solvent present was evaporated
more than three thousand years and perhaps ( Kokate C K, 2004) .
combinations of herbs must have been known since
Formulation:-
then, but now people have all along been using
synthetic medicines. The age old techniques have been Based on the sensitivity and the resistance observed by
forgotten. After studying the drawbacks mentioned MIC of the extracts formulation was prepared by using
above, people are now more aware and inclined the standard formula.
towards the use of non-alcoholic or herbal
formulations. Herbal toothpaste do not contain the Composition
artificial colors, flavours or fluoride that many of the Apple peel extract : 5.0gms
artificial products contain Lemon peel extract : 5.0gms
Orange peel extract : 5.0gms
MATERIALS AND METHOD
Banana peel extract : 5.0gms
Ingredients: Apple peel, Lemon peel, Orange peel, Carbopol 934 : 5%
Banana peel, Peppermint oil, Demineralised water. Tween - 80 : 2%
Glycerine : 1%
Apple peel- Apple fruit is botanically known as Malus
Sodium benzoate : 1%
domestica belonging to the family Rosaceae. The fruit
Sodium hydroxide : 1% sol
was procured from local market.
Clove oil : 0.5 %
Orange peel-Orange fruit is botanically known as Demineralised water : 80ml.
citrus arranticum. L. belonging to the family
Procedure:
Rutaceae. It was collected from local market.
5 gms of the apple peel extract, 5gms of orange peel
Lemon peel-Lemon fruit is botanically known as
extract, 5gms of banana peel extract , 5 gms of lemon
Citrus aurantifolia (christam& panz) swing. belonging
peel extract were triturated with 5gms of capbopol 934
to the family Rutaceae. It was procured from local
and 1 grm of sodium benzoate (as a preservative) in a
market.
motar-pestel . To it 2 ml of tween 80 was added to
Banana peel- Banana fruit is botanically known as M. remove the stickiness. Further 1 ml of glycerine was
acuminate belonging to the family Musaceae. It was added, triturated well and to it 80 ml of demineralized
collected from local market. water was added to make up the to 100gm. PH is
adjusted with a solution of sodium hydroxide. Clove
General Procedure for Extraction-The crude powder
oil is added to mask the bitter taste.
of the above peel was defatted with pet ether (40-600)
and then the defatted material was subjected to RESULTS
extraction with hydroalochol using a soxhlet apparatus.
Phyto chemical tests of the extracts were carried out
The extract was concentrated with the help of a
and the following results were observed. (table no-1) 14

TABLE 1: Results of preliminary phytochemical tests

PHYTOCONSTITUENTS APPLE BANANA ORANGE LEMON PEEL
PEEPL PEEL PEEL
Tests for Flavanoids
Flavanoids:-
a) Shinoda test + + + +
b) Alkaline reagent test
c) Lead acetate test
d)Ferric chloride test
Tests for Glycosides
Tests for Cardiac Glycosides
a) Baljet test _ _ _ _
b) Legal test
c) Keller-Killiani test
d) Liebermann's test
Tests for Anthraquinone
glycosides
a) Borntrager’s test _ _ _ _
b) Modified Borntrager's test

Test for Saponins

a) Foam test + _ + +
b) Haemolysis test
© 2011-14, JDDT. All Rights Reserved ISSN: 2250-1177 CODEN (USA): JDDTAO
Dinnimath et al Journal of Drug Delivery & Therapeutics. 2014; 4(6):68-74 70

PHYTOCONSTITUENTS APPLE BANANA ORANGE LEMON PEEL

PEEPL PEEL PEEL
Test for Terpines
a) Salkowski test + + + +
b) Libermann–Burchard test
Test for Alkaloids

a. Vitali-Morin’s test + _ + +
b. Gerrard’s test

Test for tannins

a. KOH test + + + +
b. Ferric chloride (FeCl3) test

SPECTRAL ANALYSIS OF THE EXTRACTS ( Katta V, 2005)

The extracts were studied by UV-VIS spectroscopy and FT-IR. The results are mentioned below (table 2 and 3).
TABLE 2: Results of Ultra Violet Spectroscopy

EXTRACT CONCENTRATION in mg/ml ABSORBANCE in nm

Apple peel 1mg 250

TABLE 3: Results of Infra Red Spectroscopy

Extracts Absorbance Values in cm-1 Groups present

Apple peel 2900 Aromatic CH gp
2250 Vinyl gr C=C
3400 Alcohol OH
Lemon peel 2950 Aromatic CH gp
1650 Carbonyl gr C=O
Orange peel 3350 Alcohol OH

Banana peel 3400 Alcohol OH

2950 Aromatic CH gp
1700 Carbonyl gr C=O

Ultra-Violet spectroscopy
UV spectrum was carried out by UV-SICAN 2301 for the apple peel extract by dissolving the extract 1mg/1ml in
ethanol and the spectrum has shown characteristic absorption peaks between (λmax) 200-400 nm and spectrum was
interpreted for the presence of characteristic groups and conjugation system (picture 1).

Figure 1: Ultra-Violet spectroscopy

© 2011-14, JDDT. All Rights Reserved ISSN: 2250-1177 CODEN (USA): JDDTAO
Dinnimath et al Journal of Drug Delivery & Therapeutics. 2014; 4(6):68-74 71

Infra Red spectroscopy

Analysis of the I.R spectra was carried out by IR-SHIMADZU using 1gm/ml of extract and the extracts showed the
presence of the following groups. (Picture- 2, 3, 4, 5)

FIGURE 2: IR Spectrum of Apple peel extract

FIGURE 3: IR Spectrum of Lemon peel extract

© 2011-14, JDDT. All Rights Reserved ISSN: 2250-1177 CODEN (USA): JDDTAO
Dinnimath et al Journal of Drug Delivery & Therapeutics. 2014; 4(6):68-74 72

FIGURE 4: IR Spectrum of Orange peel

FIGURE 5: IR Spectrum of Banana peel

© 2011-14, JDDT. All Rights Reserved ISSN: 2250-1177 CODEN (USA): JDDTAO
Dinnimath et al Journal of Drug Delivery & Therapeutics. 2014; 4(6):68-74 73

HPTLC study of extract

High-performance thin-layer chromatographic (HPTLC) analysis of the apple peel extract was carried out using
Anchrom-HPTLC with CAMAG Scanner. The separation was carried out on a TLC aluminium plates precoated with
silica gel 60F-254 as the stationary phase, eluted with chloroform–ethylacetate–formic acid (2.5 : 1 : 0.1) as mobile
phase. This system was found to give compact spot for trans-resveratrol (Rf value of 0.40_0.03) ( Fig 6).

FIGURE 6: High-performance thin-layer chromatographic (HPTLC) analysis of the apple peel extract

Linear ascending development was carried out in 20 and 400 nm ( picture (1) (table no-2) . These correspond
cm_10 cm twin trough glass chamber (Camag Muttenz, to conjugated dienes present in the extracts. Later, the IR
Switzerland) using mobile phase consists of chloroform– spectra of the extracts have shown the presence of
ethylacetate–formic acid (2.5 : 1 : 0.1). The length of alcoholic OH groups, carbonyl groups and CH-aliphatic
chromatogram run was 8 cm. Subsequent to the groups and vinyl group (C=C) in them at their
scanning, TLC plates were air dried and scanning was characteristic values (fig -2,3,4 and 5)(table 3). HPTLC
performed on a Camag TLC scanner III in absorbance analysis of the apple peel extract has also shown the
mode at 313 nm and operated by Cats software 4.03 presence of vital constituents. As these Polyphenolic
version. Evaluation was via peak areas with linear compounds are found to be present in these plant
regression ( Katta VK, 2005). extracts, they may be responsible for the activity.
CONCLUSION
A study effort has been made for preparing a new
Polyherbal toothpaste by combining the active
constituents of the different extracts to for tooth decay.
For the present study, apple, lemon, banana, orange were
subjected for extraction and these extracts were used for
the a new polyherbal toothpaste with anti-microbial
efficacy. The extracts of apple, lemon, and banana,
resveratrol orange, peels were studied for the phyto constituents
present in them by phytochemical tests followed by
DISCUSSION spectral study like UV, IR and HPTLC study.
The preliminary Phytochemical investigations of the ACKNOWLEDGEMENT:
extracts have revealed the presence of important groups
(Table 1) such as steroids, alkaloids, terpenoids, Authors acknowledge the financial support provided by
flavanoids, tannins and saponins. The spectral data Science and Technology dept, Govt of Karnataka ( Vgst-
carried out by UV-VIS spectroscopy and FT-IR also has spice program) for the present research work. Authors
confirmed the presence of these active constituents in the also thank Principal, KLEU’S College of Pharmacy
extracts. The UV-VIS spectra of extracts shown Belgaum for providing all necessary support for the
characteristic absorption peaks between λmax- 200 nm research work.
© 2011-14, JDDT. All Rights Reserved ISSN: 2250-1177 CODEN (USA): JDDTAO
Dinnimath et al Journal of Drug Delivery & Therapeutics. 2014; 4(6):68-74 74

REFERENCES
1. Abdulwahab I, Al-Kholani. Comparison between the Efficacy 9. Shyamala B, Nagarajaiah and Jamuna P. Chemical
of Herbal and Conventional Dentifrices on Established composition and antioxidant potential of peels from three
Gingivitis. Dent Res J, 2011; 8(2): 57-63 varieties of Banana. As. J. Food Ag-Ind. 2011; 4(01):31-46
2. Wolfgang Weinert in "Oral Hygiene Products" Ullmann's
Encyclopedia of Industrial Chemistry, 2005, Wiley-VCH, 10. Marie LL et a. Volatile Components of Peel and Leaf Oils of
Weinheimdoi:10.1002/14356007.a18_209: Lemon and Lime species. J. Agric. Food Chem 2002; 50:
3. http://www.mind-mart.com/oral-hygiene/benefits-of-herbal- 796-805
toothpaste[Accessed 08 Jan 2013]. 11. Hegazy AE et al. Antioxidant Activities of Orange Peel
4. Perlich MA, Bacca LA, Bollmer BW, Lanzalaco AC, Extracts. World Applied Sciences Journal 2012;18 (5): 684-
McClanahan S, Sewak LK, Beiswanger BB, Eichold WA. 688
The clinical effect of a stabilized stannous fluoride dentifrice 12. Kokate CK S.B.Ghokale . Pharmacognosy 47thedition 2012,
on plaque formation, gingivitis and gingival bleeding: a six- Nirali Prakashan.pg no 8.3
month study. The J of Clinical Dentistry, 1995; 6: 54–58. 13. Handa SS et al. 2008. Extraction Technologies for Medicinal
PMID 8593194 and Aromatic Plants, International Centre for Science and
5. Debjit B, Sampath Kumar KP, Akhilesh Y, Shweta S, High Technology, Trieste Pak. J. Bot., 43: 63-67, Special
Shravan P, Amit SD. Recent Trends in Indian Traditional Issue, December, 2011 (Medicinal Plants: Conservation &
Herbs Syzygium Aromaticum and its Health Benefits. J of Sustainable use)
Pharmacognosy and Phytochemistry, 2012 14. Khandelwal KR, Techiniques and experimental textbook of
6. Wolfe K. Antioxidant activity of apple peels. J Agric Food Practical pharmacognosy 9 th edition 2002., Nirali
Chem, 2003; 51(3):609-614. Prakashan; : pg no 149-156
7. Diankov S, Karsheva M, Hinkov I. Extraction of natural 15. Katta Vijaya kumar et al estimation of trans-Resveratrol in
antioxidants from lemon peels. kinetics and antioxidant Herbal Extracts and Dosage Forms by High-Performance
capacity. J of the University of Chemical Technology and Thin-Layer Chromatography Chem. Pharm. Bull. 53(6) 691—
Metallurgy, 2011; 46(3):315-319 693 (2005).
8. Zia-ur-Rehman. Citrus peel extract–A natural source of
antioxidant. Food Chemistry, 2006;99(3): 450–454

© 2011-14, JDDT. All Rights Reserved ISSN: 2250-1177 CODEN (USA): JDDTAO