Validation f Reported Analytical Method for Evaluation Of

7/28/2019 Validation f Reported Analytical Method for Evaluation Of

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VALIDATION OF REPORTED ANALYTICAL

METHOD FOR EVALUATION OF DIFFERENTBRANDS OF DICLOFENAC SODIUM

Prepared by:Patel Himani N.

B.Pharm sem-VIII

Roll no-34

K.B.I.P.E.R


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PROPERTIES OF DICLOFENAC SODIUM

THERAPEUTIC CLASS: Nonopioid

analgesic, antiarthritic

STRUCTURAL FORMULA:

C14H10Cl2NNaO2MELTING POINT:: 284C

PROTEIN BINDING:99.5%

HALF LIFE: 1.2-2hr

METABOLISM: Hepatic glucuronidation

and sulfoxidation

EXCRETION: urine(65%)&feces (35%)ROUTE:oral,topical,i.v.,transdermal


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MECHENISM OF ACTION

The anti-inflammatory effect of diclofenac sodium arebelieved to be due to inhibition of leukocyte migration&the enzyme cyclooxygenase (COX1&2) leading toperipheral inhibition o prostaglandin synthesis. It also

appears to exhibit bacteriostatic activity by inhibitingbacterial DNA synthesis.

As prostaglandins sensitize pain receptor,inhibition of theirsynthesis is responsible for analgesic effect ofdiclofenacsodium.

Antipyretic effect may be due to action on thehypothalamus resulting in peripheral dilation increasedcutaneous blood flow &subsequent heat dissipation.


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ADVERSE EFFECT

Stomach pain

Constipation

Diarrhea

Heartburn or indigestion (dyspepsia) Gas

Unexplained bleeding

Ulcer in the stomach or intestines (peptic ulcer)

Nausea Vomiting

Anemia


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MEDICAL USE

Pain

Inflammatory disorders

Dysmenorrhea

Rhumatoid arthritis

Polymyositis

Pain management in case of kidneystone&gallstone

Acute migraine

Post-operative pain

Peptic ulcer


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UV VISIBLE SPECTROSCOPY

PRINCIPLE OF UV SPECTROSCOPY

Molecules containing -electrons or non-bonding

electrons (n-electrons) can absorb the energy in the form of

ultraviolet or visible light to excite these electrons to higheranti-bonding molecular orbitals. The more easily excited the

electrons (i.e. lower energy gap between the HOMO and the

LUMO), the longer the wavelength of light it can absorb


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The absorption of radiation is governed by mainly two laws,

1) Beers law (Related to concentration of absorbing species)

2) Lambertslaw (Related to thickness/path length of absorbing species)

Beers law:

It states that the intensity of a beam of monochromatic light deceasesexponentially with increasing the concentration of absorbing species.

Lamberts law:

It states that the intensity of a beam of monochromatic light with thethickness of the medium is directly proportional to the intensity of incidentlight.


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Instrumentation

A. Basics of the Instrumentation

A spectrometer is an optical system that transmits a specific bandof electromagnetic spectrum. Dispersion of different wavelengthsis accomplished with the separating capability of refraction(prism) or diffraction (diffraction grating). Typical applications are

isolation of a narrow band of radiation from a continuum lightsource for absorption measurements, or analysis of the emissionfrom excited atoms or molecules.


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TYPE OF PHOTOMETER

Single Beam Spectrophotometer

Dual Beam Spectrophotometer


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ICH GUAIDLINE OF VALIDATION

ICH parameter of validation

1. Acurracy

2. Specificity

3. Precision

4. Range

5. Quantitation limit

6. Detection limit

7. Linearity


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LINEARITY

Peparation of standaed stock solution

Diclofenac sodium standard 50mg was taken &made the volume 100ml

with 0.01N NaoH.sonicated for 10min,Filtered the solution &took 2ml of

Filtered solution&made the volume 100ml with 0.01 N NaoH.For

spectrophotometric method for standard preparation,0.01N NaoH Wasreplaced with Methanol.

Linearity

From the standard stock solution 0.2ml, 0.3ml, 0.4ml, 0.5ml, 0.6mldilutions were made in 10ml volumetric flask and volume was made up to

the mark with methanol to obtain concentration in range of 10-30g/ml.

The spectra were recorded, absorbance were measured at 282nm and

calibration curve was plotted.


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ACURRACY

For the study of the accuracy level of recovery in done at

80%,100%,120% for this 20 g/ml test solution is

prepared,for the recovery study add respectively 16

g/ml,20 g/ml, 24 g/ml solution of the standard drug ofdiclofenac sodium.measure the absorbance of resulted

solution at 282 nm against a reagent as blank.

Precision

I. Interday precision

II. Intraday precision


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INTERDAY PRECISION

For the study of the interday precision prepare a

solution of 10g/ml,20g/ml,30g/ml of the standard

drug solution at the interval of 0 hrs ,2 hrs,

4hrs.measure the absorbance at 282 nm againstreagent as blank.

INTRADAY PRECISION

For the study of the intraday precision prepare a

solution of 10g/ml,20g/ml,24g/ml of the standarddrug solution at the interval of day1,day2,

day3.measure the absorbance at 282 nm against

reagent as blank.


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LOD AND LOQ

Detection Limit

The detection limit of an individual analytical procedure isthe lowest amount of analyte in asample which can bedetected but not necessarily quantitated as an exact value.

LOD=10/sQuantitation Limit

The quantitation limit of an individual analytical procedure isthe lowest amount of analyte ina sample which can be

quantitatively determined with suitable precision andaccuracy.

LOQ=3.3/s


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COUNCLUSION

The proposed method for evaluation of different

brands of diclofenac sodium is suitable technique &

could be applied for the routine analysis in quality

control laboratories.


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THANK YOU

Validation f Reported Analytical Method for Evaluation Of

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