Qualitative Determinations of Steroids in Face Cream Formulation by Fourier Transform Infrared Spectrometry

 

Agarwal Alka1*, Ashawat M.S.1, Sharma K.1, Bele D2 and Singhvi I.J1

1Pacific College of Pharmacy, Udaipur (Raj.)

2Charak Institute of pharmacy, Mandleshwar, Khargone (M.P.)

*Corresponding Author E-mail: alkaagarwal2007@rediffmail.com

 

ABSTRACT:

Topical steroid application is associated with adverse effects especially if they are used incorrectly. The risk of most of the side effects depends on the strength of the steroid, the length of application, the site treated, and the nature of the skin problem.

In present investigation, randomly selected cosmetic cream formulations (According to the ingredients mentioned on the label with none of the information about steroidal components) of repute brands (Users choice) from market. All procured and selected formulations were coded as (M1-M18) for the purpose of psychometric, physicochemical and chemical analysis. The results of chemical analysis showed that, among 18 cream formulations eight formulations were found to be positive for presence of steroids. After the chemical analysis positive selected 08 (M2, M4, M6, M7 , M8, M13, M16, M18) decoded formulations were further selected for  authentic specific qualitative analysis by using a zinc selanium Fourier transform infrared spectroscopy, which was used for the determination of steroidal adulteration in cosmetics cream formulations and obtained IR spectra were compared with standard Prednisolone steroidal preparation.  From the result of IR spectra it was evident that many marketed formulation which promises instant fairness, glowing, brighten skin may have a dreadfully negative and serious side effect on the skin due to presence of steroid.

 

KEYWORDS: Steroids, Inflammation, Cream formulations, Psychometric, Physicochemical, IR spectra.

 


 

INTRODUCTION:

Redness, erythema and dermatitis or eczema is a common dermatological disorder affecting most of the population and is the nearly every one skin condition in our country. Topical formulations such as creams or ointments, lotion applied multi times daily are considered the most appropriate therapy for the treatment of such conditions. The topical steroids are however considered for the majority of users and as a consequence the use of white petroleum and hydrogenated vegetable oil as supplemental therapy is usually required1. Steroidal compositions for external use can relieve inflammation but treat so many skin ailments. Topical steroids have revolutionized the practice of dermatology since they were introduced in the late 19502. They are prescribed as anti-inflammatory preparations used to control so many other skin conditions3.

 

Chronic use of topical steroidal creams is known to cause thinning of the skin (atrophy), which sometimes results in permanent stretch marks (striae), swelling of fine blood vessels (telangiectasia), perioral dermatitis (rash around the mouth), enlarged blood vessels (telangiectasia) and temporary loss of pigment in the areas of skin treated. Further it enhances susceptibility of a person to skin infections, skin allergies, making the eczema appear to get worse. Like all medications, topical cortico steroids are associated with potential adverse effects (side effects) especially if they are used incorrectly4,5.

 

In the present research segment the widely used different topical cream formulations were randomly selected from market. According to the compositions of selected marketed cream formulations which were mentioned on the label, it was not providing any information about steroidal presence in preparation. Adverse reaction in users produced by so many marketed tropical preparations. We have evaluated different marketed preparation for the presence of steroid firstly by qualitative test6 and then reevaluated by FTIR spectroscopy.

 

 

The objectives of this work is to observe specific marker adulteration data of marketed cosmetic cream  formulations, starts from qualitative analysis to finger printing estimation by FTIR for  screening of steroidal adulteration in formulations.

 

MATERIALS AND METHODS:

Chemicals: All chemical and solvents used were of analytical grade.

(1)                 Selection of Formulation: The cream formulations were selected based on a user’s choice questionnaire filled by 78 persons. The persons were of different socio economic status, age of both genders with different working area.

 

(2)                 Decoding of Formulations: All randomly selected cosmetic cream formulations of repute brands (Users choice) from marked were coded by Marketed Formulations (M1-M18) for the purpose of psychometric and physicochemical testing7.

 

(3)                 Psycometric Analysis: The selected cosmetic cream formulations were firstly evaluated for their psychometric analysis by using panel of subjective blind procedure (12 subjects in the age gr. of 22-25 years includes both genders previously trained for cosmetic terminology), each decoded formulation were pass through the each subject in circulation8-9.

 

(4)                 Chemical Analysis of Creams: Standard chemical reactions viz.  Salkowaski reaction, Lieberman Bruchard reaction and Lieberman reaction were used to detect the presence or absence of steroids in various selected face creams in following manner.

Ø     Salkowaski reaction:  A small quantity of cream was dissolved in 2ml of chloroform; to that 2ml concentrated sulphuric acid was added. After shaking well, red chloroform layer appears and acid layer show greenish yellow color, if steroid is present.

Ø     Lieberman Bruchard reaction: A small quantity of cream was dissolved in 2ml of chloroform. Then added few drops of acetic anhydride and conc. H2SO4. First red then blue and finally green color are appears, if steroid is present.

Ø     Lieberman reaction: A small quantity of cream was dissolved in 3ml of chloroform. Then added 3ml of acetic anhydride. Heated and cooled the prepared solution. Then added few drops of conc. H2SO4. As a result a blue color is appears 10 if steroid is present.

 

(5)                 IR Spectroscopy: The infra-red (IR) absorption spectrum of serially coded cream and lotion formulations were determined using Zinc solenoid (ATR) FTIR spectrophotometer Bruker Tensor-27 model.

 

RESULT AND DISCUSSION:

The psychometric evaluation of all selected cream formulations shows unremarkable results and lying in satisfactory criteria. The results are shown in table 1 suggest that the formulation (M2,M5,M7,M8,M13) are in poor subjective spread ability criteria as well as the formulations(M1,M11,M14,M18) showing the poor pickup by the subjects panel, the results are summarized in table 1. The second step of experiment is qualitative analysis of test formulations by using official procedure of specific steroidal functional group determination. The official chemical analysis reactions e.g. Salkowaski reaction, Lieberman Bruchard reaction and Lieberman reaction were performed to detect the presence or absence of steroids in various selected creams formulation. The results of chemical analysis showed that, among 18 cream formulation eight formulations were found to be positive for presence of steroids (table no 2). After the chemical analysis positive selected 08 (M2, M4, M6, M7 , M8, M13, M16, M18) decoded formulations were further selected for next step. The third step of experiment was carried for authentic specific qualitative analysis by using a zinc selanium Fourier transform infrared spectroscopy, which was used for the determination of steroidal adulteration in cosmetics cream formulations. After preliminary qualitative reaction based analysis the presence of different constitute in various market coded cream formulations were determined by IR spectroscopy and compared with IR spectroscopy of the pure steroidal Prednisolone preparation. All the suspected formulations were pulled for comparison of data obtained from infrared spectroscopy. The IR spectra are shown in Fig-1-6 Suggest that marketed cream formulations ((M2, M4, M6, M7, M13, M18) test samples have been adulterated with prednisolone steroidal moiety. The results of steroid presence in analyzed decoded formulations showed in M2 is justify because it already labeled the content of Clobetasol as purposely use cream prescribed by doctors for treatment of  dermatitis.

 

Fig1: Sample M2 containing (Clobetasol) with Pure steroid

 


Table no. 1: The results of psychometric and preliminary analysis

Formulation Code

pH

Acid value

Spread ability

Color

Gloss

Pickup

Residue remain

M1

6.11±0.03

9±0.1

+

Creamy white

-

+

M2

6.23±0.02

8±0.9

-

Milky white

+

++

M3

5.94±0.03

8±0.2

+

Pinkish

+

+

M4

6.33±0.02

9±0.1

+

White

+

+

M5

5.99±0.03

9±0.2

-

Creamy white

+

+

M6

6.37±0.02

8±0.6

+

Creamy white

+

++

M7

6.43±0.02

9±0.1

-

Milky white

+

+

M8

6.39±0.03

9±0.1

-

Pinkish

+

+

M9

5.79±0.03

8±0.9

+

Creamy white

+

-

M10

5.93±0.02

8±0.2

+

Creamy white

+

+

M11

5.09±0.02

7±0.1

+

Milky white

-

-

M12

5.99±0.02

9±0.2

+

Pinkish

+

+

M13

6.33±0.04

8±0.6

-

Creamy white

+

+

M14

5.96±0.02

9±0.1

-

Milky white

-

+

M15

5.97±0.03

9±0.9

+

Pinkish

+

+

M16

6.36±0.02

8±0.9

+

Creamy white

+

+

M17

6.03±0.02

8±0.2

+

Yellowish

+

+

M18

6.33±0.03

9±0.1

-

Milky white

-

-

-: Poor, +: Good and accepted by panel, ++: Remarkable, +++: not accepted

 

 


 

Fig 2: Sample M4 with Pure steroid

 

Fig 3: Sample M6with Pure steroid

 

Fig 4: Sample M7with Pure steroid

 

Fig 5: Sample M13with Pure steroid

 

Fig 6: Sample M18with Pure steroid

 

Table no. 2: The results of chemical analysis:

S. No.

Marketed decoded formulations

Salkowaski reaction

Liberman Bruched reaction

Liberman reaction

1.

M1

_

_

_

2.

M2

+

+

+

3.

M3

_

_

_

4.

M4

+

+

+

5.

M5

_

_

_

6.

M6

+

+

+

7.

M7

+

+

+

8.

M8

+

+

+

9.

M9

_

_

_

10.

M10

_

_

_

11.

M11

_

_

_

12.

M12

_

_

_

13.

M13

+

+

+

14.

M14

_

_

_

15.

M15

_

_

_

16.

M16

+

+

+

17.

M17

_

_

_

18.

M18

+

+

+

 

The infra-red (IR) absorption spectrum of serially coded cream and lotion formulations  were determined using Zinc solenoid (ATR) FTIRspectrophotometer and the resultant spectrum are shown in Comparative  IR absorption spectrum which shows principal peaks at wave-numbers 1666, 1612, 1724, 1063 and 1010 cm-1 and the relevant band assignments determined using theoretical concepts are summarized in the below table-3.

 

Table no. 3: The results of IR Spectroscopy:

Band position (cm-1)

Assignment

1666

C=C stretching of the aliphatic non-conjugated alkene

1612

C=O stretching of the ketone

1724

C-Cl stretching of chlorine

 

1063

COO stretching of the ether

1010

O-H bending of the alcohol

 

Such results show the presence of   topical steroids which are generally believed to have anti-inflammatory, anti-proliferative, anti-puritic, and vasoconstrive properties. The serious side effects nearly always follow the formulations of uncontrolled repeating use and have been reported more frequently for the treatment of psoriasis than in eczema, probably due to the fact that the parakeratotic keratin of psoriatic skin is more permeable than normal keratin. The adverse effects of such are so many times noticed as localized skin reactions occurring at the site of application and generalized adverse effects arising from systemic absorption of the compound also.

 

CONCLUSION:

From this short research projects segment, we conclude that all marketed preparation which promises instant fairness, glowing, brighting skin may have a dread full negative side and may show serious side effect on the skin. The longer use of such cosmetic creams preparations may leave the dangerous impact on the all kind of skin.

 

 

REFERENCES:

1.        Bull. Alex. Fac. Med. 42 No. 1 (supplement), 2006.

2.        Del Guidice P, Raynaud E, Mahe A. Cosmetic use of skin depigmentation products in Africa. Boc Pathol Exot 96 (5); 2003 Jan: 389-93.

3.        Hengge U.R, Ruziicka T. and Schwartz R.A. “Adverse effects of topical glucocorticosteroids.” J Am Acad Dermatol. 54(1); 2006: 1-15.

4.        Witzmann and Rupert. “Steroids: Keys to life.” New York: neither Van nor strand Reinhold Co., 1977.

5.        Long C.C and Finlay A.Y. “Perceived under prescription of topical therapy.” Br J Gen Pract. 43(372); 1993: 305.

6.        Agarwal A., Singhvi I.J., Bele D., Sharma K., Gupta S.K., Karwani G.and Kumawat M. Evaluation of steroids in face creams of different marketed brands. IJPT 3(2); 2011:| 2480-2486.

7.        Ashawat M.S., Saraf Swarnlata, Saraf Shailendra. Herbal cream cosmetic formulations for the improvement of skin viscoelastic properties. International journal of cosmetic sciences. 3; 2008: 82-93.

8.        Ashawat M.S., Saraf Swarnlata, Saraf Shailendra. Cosmetic potentiality of plant extracts and natural oils, journal of bioscience biotech. Res. Asia, 3(ia); 2006: 181-188.

9.        Ashawat M.S., Saraf Swarnlata, Saraf Shailendra. Biochemical and histopathological study of herbal cosmetic cream formulation. International journal, trends in medical research (New York academic press), 2, 3; 2007:135-141.

10.     Khandelwal K.R. “Practical Pharmacognocy.” Nirali Prakashan (18th edition):151.

 

 

 

 

 

Received on 23.05.2011          Modified on 03.06.2011

Accepted on 10.06.2011         © RJPT All right reserved

Research J. Pharm. and Tech. 4(10): Oct. 2011; Page 1547-1550