VALIDATION OF IBUPROFEN AND PARACETAMOL IN

BINARY MIXTURES USING UV SPECTROPHOTOMETRIC

METHOD
DEPARTMENT OF PHARMACEUTICAL ANALYSIS

GROUP MEMBERS:
[Link] (06Q11R0012)
[Link] (06Q11R0027)
[Link] (06Q11R0041)
[Link] (06Q11R0019)

UNDER THE GUIDANCE OF

Mr. [Link], [Link]., (Ph.D)

SRI LAKSHMI NARASIMHA COLLEGE OF PHARMACY

OBJECTIVE OF THE STUDY

• There is no official specific spectrophotometric method for the estimation of drug

combinations Ibuprofen and Paracetamol in binary mixtures.

• The HPLC, HPTLC, UV spectrophotometric methods are available for estimation of this
combination.

• The HPLC, HPTLC methods are expensive and complicated. So we developed the rapid,
simple, UV spectrophotometric method of estimation of Ibuprofen and Paracetamol in oral
dosage formulations without any previous separations.
INTRODUCTION
 Analytical monitoring of a pharmaceutical product is necessary to ensure its safety,
efficacy throughout all phases of its shelf life including storage.
 In this project, UV spectrophotometric method was developed for the estimation and
validation of Ibuprofen and Paracetamol in combined oral dosage forms without
previous separation.

Ultraviolet-Visible spectrophotometry involves the measurement of amount of

ultraviolet(190-380nm) or visible(380-800nm) radiation absorbed by a substance in a
solution
 Validation means “Assessment of validity” or “Establishing the documented
evidence which provides a high degree of assurance that a specific process will
consistently produce a product of predetermined specifications quality attributes.

 The solvent selected by performing their solubility study in various solvents.

 LITERATURE SURVEY
 Wafaa [Link], department of Analytical chemistry, proposed “Determination of Ibuprofen and Paracetamol in
binary mixture using chemo metric-assisted spectrophotometric methods”

 Ranjana soni [Link] proposed “Spectrophotometric Methods for Simultaneous Estimation of Dexibuprofen and
Paracetamol”

 Prasanna Reddy Battu and MS Reddy proposed “RP-HPLC Method for Simultaneous Estimation of
Paracetamol and Ibuprofen in Tablets”

 Bhatia M.S. kashedikar,S.G.,and chaturvedi, proposed “Development of the second-order derivative UV

spectrophometric Method for direct determination of Paracetmol in urine intented for Biopharmaceutical
Characterization of drug products”

 Munde,D., and kaskhedikar, S.G., Estern pharmacist proposed “simultaneous LC determination of Paracetamol
and related compounds in Pharmaceutical formulations using a C based column”

 Jhawala, J.L.,Sothi,R.A., and Sane(R.T., Indian drugs) proposed “HPLC assay of acetylsalicylic acid,
Paracetmol, Caffeine and Phenobarbital in tablets”

 Sothi, R.A., Chawala,J.L. and Sane,proposed “HPLC assay of acetylsalicylic acid, Paracetmol, Caffeine and
Phenobarbital in tablets”
PLAN OF WORK

Study of solubility of the drug in different solvents.

Determination of λmax for the sample

Calibrated graphs were to be established in range of 5-100 and 10-100µg/ml for Ibuprofen and
Paracetamol at wavelength 320 to 380nm which shows maximum absorbance

Beer’s law has to be verified.

Estimation of pharmaceutical dosage form (combination of Ibuprofen and Paracetamol)

without any Previous separations

All of the above proposed methods have to be extensively validated

 EXPERIMENT
Preparation of standard solutions and calibration
Stock standard solutions containing 0.5 and 1.0 mg ibuprofen and paracetamol respectively, were dissolved
in 10 ml ethanol.

Standard solutions of both drugs were prepared individually by dilution of the stock solutions with ethanol to
obtain concentration range of 0.1 – 0.5 μg mL-1 for Ibuprofen and Paracetamol

These are measured at wavelength 320 nm to 380 nm and the corresponding absorbances are noted for
the estimation of Ibuprofen and Paracetamol.

The above noted absorbances of standard Ibuprofen and Paracetamol follows Beer’s law .
Analysis of pharmaceutical dosage form

10 tablets labeled to contain 400mg of ibuprofen and 325 mg of paracetamol were powdered.

Accurately weigh powdered tablet of about 950mg , transferred into a 100 mL calibrated flask, diluted with
ethanol, stirred for about 10 min and then make up the volume with the same solvent.

This solution was heated gently and filtered to remove any insoluble matter.

After filtration, working solutions were prepared by transferring suitable aliquots of clear filtrate and diluting
with appropriate solvent.

These were measured at wavelength 320 nm to 380 nm and the corresponding absorbances are noted for
the estimation of Ibuprofen and Paracetamol in combined dosage form without any previous separations.

From the above noted absorbances shows that the pharmaceutical dosage form also follows Beer’s law.
Method of Validation : Some of the parametres has been validated. They are

ACCURACY: Relates to the closeness of test results to true value which is expressed as percentage
recovery by assay of known/added amount of analyte in linearity range.

RECOVERY STUDIES: These studies were carried out by the standard addition method.

LINEARITY: Ability of the method to elicit test results that are directly proportional to the concentration of the
analyte.

PRECISION: Degree of agreement among individual test results when procedure is applied usually
expressed as SD/RSD. It includes
a)Repeatability: Experiment done under same conditions (same analyst, same test method and under same
set of laboratory conditions) within short interval of time.

a)Reproducibility: Experiment done under different conditions i.e. carried out by different analysts in different
laboratories using different equipments on different days.


Results: DETERMINATION OF λmax

Content Uniformity
Equivalent Label Amount of Percentage
[Link]
weight taken Claim(mg) Drug(mg) purity (%W/W)

1. 940mg 725 281.02 86.46

2. 940mg 725 282.82 87.02

3. 940mg 725 280.17 86.2

4. 940mg 725 274.86 84.57

Mean =86.05


Accuracy
Label claim per % label claim estimated % CV % RSD Standard
Formulation (mean ±standard deviation)
Per tablet (mg) Error

Sample 725 86.05± 1.056 0.4184 1.98 0.528

Recovery studies
Amount of drug in pre Standard % Recovery Standard
analysed Tablet powder Bulk Drug Estimation % CV

(Ibuprofen+ (mean±S.D) error

(mg)
Paracetmol)

940 30+30 91.15± 4.19 5.84 2.42

940 60+60 119.3± 4.5 6.744 2.60

940 120+120 165± 5.20 9.0 3.0



Linearity

S. No Concentration Absorbance at max 320nm

1. 0.1g / ml 1.25

2. 0.15g / ml 1.9

3. 0.2g / ml 2.56

4. 0.25g / ml 3.2

5. 0.3g / ml 3.8
Precision

Formulation Label claim per % label claim estimated % c.o.v % R.S.D Standard

Per tablet (mean +standard Error

deviation)
(mg)

1. 725 86.05+1.056 0.4184 1 0.528

2. 725 85.75+0.96 0.35 1 0.48

 Discussion

 Solubility study of Ibuprofen and Paracetmol were performed in various solvents and solvent
selected is ethanol.

 Sample which is a combination of Ibuprofen and Paracetmol diluted in ethanol shows maximum
absorbance at 320nm to 380nms.

 The proposed method is a spectrophotometric method for determination of Ibuprofen and

Paracetmol in combined oral dosage forms without previous separations.

 Beer’s law and linear regression equations were verified.

 Validation of the proposed methods developed by statistical analysis of the results obtained for
the suggested measurements are equally precise and accurate to the reported methods.
CONCLUSION:

 The UV Spectrophometric methods enable the quantitation of Ibuprofen and Paracetmol

binary mixtures with good accuracy and precision, either in laboratory prepared samples or
in Pharmaceutical dosage forms.

 The good recoveries obtained in all cases as well as the reliable agreement with the reported
procedure proved that the proposed methods could be applied efficiently for determination
of Ibuprofen and Paracetmol in Binary mixtures with quite satisfactory precision.

 It could be easily used in a quality control laboratory for their analysis.

 This method is simple and rapid.

REFERENCES
1. Beckette A.H and Stenlake J.B. “Practical Pharmaceutical Analysis”. 4 th edition P. No. 275 – 325.

2. Skoog “Fundamental of Analytical Chemistry”, West Holler and Enough. P. No. 707.

3. ICH, Q2 (R1) “Validation of Analytical Procedures:Text and Methodology” (2005) International Conference
on Harmonization.

4. CIMS current index of Medical specialties CIMS-101 April-July 2008 [update-2]and Drug [Link]., Drug
Information Portals.

5. Indian Pharmacopoeia. 1996 Vol I & Vol II P. No. 7, A –76, 77, 169, 192 Ministry of health and welfare
science- New Delhi.

6. Wafaa [Link], department of Analytical chemistry, “Determination of Ibuprofen and Paracetamol in

binary mixture using chemo metric-assisted spectrophotometric methods.” American Journal of Applied
Sciences 5 (8): 1005-1012, 2008, ISSN 1546-9239

7. Ranjana soni [Link] “Spectrophotometric Methods for Simultaneous Estimation of Dexibuprofen and
Paracetamol” Asian J. Research Chem. 2(1): J an.-March, 2009, ISSN 0974-4169.

8. Prasanna Reddy Battu and MS Reddy “RP-HPLC Method for Simultaneous Estimation of Paracetamol and
Ibuprofen in Tablets” Asian J. Research Chem. 2(1): Jan.-March, 2009, ISSN 0974-4169