Determination of pka of the given drug sample

INTRODUCTION: Dissociation constant of a drug/compound is commonly refered to as pKa. It is a characteristic of drug. It is the estimation of ionized and unionized drug concentration at a particular pH. It is the pH at which 50% of drug is ionized and 50% is unionized. The dissociation constants of both acidic and basic drugs are expressed by pKa values. The importance of pKa is that one can easily conclude how much drug is ionized and unionized. Unionized drug is better absorbed. pKa can be calculated by following equation. pKa = pH +log(di –d/ d- dm) Where, di = absorbance of the ionized species. d = absorbance of solution tested. dm = absorbance of the unionized species. U.V. spectroscopy is widely used in pKa determination as we know lambda max is different for ionized and unionized drug or we can say that there is great difference between absorbance of ionized and unionized drug at a particular lambda. MATERIALS & METHODS: Materials: Apparatus: 10 ml volumetric flasks, beaker, pipette (10 ml),spatula. Chemicals: 0.2 M Sodium hydroxide, 0.2 boric acid, 0.2 M potassium hydrogen phthalate, 0.2 M hydrochloric acid, 0.2 M potassium chloride, distilled water, test drug. Instruments: Weighing Balance, SIMADZU UV-Visible Spectrophotometer, pH meter.

Procedure for the determination of pka of given drug: 1. The absorbance values at that wavelength were noted and pka was determined from the graph between absorbance and pH. 3. .56 ml of 0.2 M Sodium hydroxide Preparation of primary stock: 10 mg of drug was accurately weighed and dissolved in 10 ml of 7:3 = methanol: water mixture as solvent to get concentration of 1 mg/ml. 1 mL ( 200 mcg/ml) of secondary stock solution was taken in each of the 9 tarson tubes. 5.9 ml of 0.2 M Sodium hydroxide (7) pH 8 : 5ml of 0.Preparation of buffers: Following buffers were prepared as per IP 2007.2 M potassium hydrogen phthalate + 0.2 M Sodium hydroxide (5) pH 6 : 5 ml of 0.2 M potassium chloride + 0.2 M potassium hydrogen phthalate + 2. 4. (3) pH 4 : 5 ml of 0.26 ml of 0. pH.39 ml of 0.2 M hydrochloric acid (4) pH 5 : 5 ml of 0. 6. All the solutions were immediately scanned in UV range.2 M Sodium hydroxide (6) pH 7 : 5 ml of 0.2 M potassium hydrogen phthalate + 0.01 ml of 0. 2. They were diluted to 10 mL with each of the pH solutions to get a concentration of 20 mcg/ml.2 M potassium hydrogen phthalate + 2.2 M boric acid + 5 ml of 0. Derivative graph was plotted by taking (∆Abs/∆pH) vs. All the spectrums were overlayed and the suitable wavelength for determination of pka was identified. Preparation of secondary stock: 2 ml of the primary stock was taken and diluted to 10 ml with 7:3 = methanol: water mixture as solvent to get concentration of 200 mcg/ml.

5229 0.0226 0.0448 0.0777 0.4683 0.2592 0.4708 303 nm ∆Abs/∆pH Abs 0.019 0.5181 0.4399 pH 2 3 4 5 6 7 8 9 10 ∆Abs/∆pH 0.468 0. 296 nm Abs 0.0563 0.4707 0.5095 0.455 0.01 0.4824 0.3851 0.568 0.436 0.0201 0.5651 0.0053 0.0223 0.0571 0.0115 0.0274 0.4736 0.0413 0.0215 0.1 0.0166 0.0336 0.4909 0.1244 0.1768 0.0036 0.0436 0.5629 0.0807 0.0158 0.4318 0.508 0.0893 0.4788 300 nm ∆Abs/∆pH Abs 0.029 0.5014 0.0437 0.0308 Plot of absorbance vs pH and its derivative graph (∆Abs/∆pH vs pH) were ploted at selected wavelengths as shown below.RESULTS AND DISCUSSION: The following table gives the absorbance values at 300 nm different pH values. 296 nm: .4541 0.2156 0.

3 0.1 0 5 pH 10 15 300 nm: H p / s b A ∆ .A b s vs p H 0 .4 0.3 0 .6 0 .5 0 .1 0 -0.1 0 2 4 6 pH 8 10 12 e c n a r o s b A ∆Abs/∆pHvs pH 0.2 0.4 0 .1 0 -0 .2 0 .6 0.5 0.

.7 0 .2 0 .1 0 0 2 4 6 pH 8 10 12 0.4 0.4 0.5 0 .6 0.2 0.1 0 H p / s b A ∆ 0 .3 0 .3 0.2 -0.3 0.4 0 .2 0.6 0 .1 0 0 5 pH 10 15 The peak in the derivative graph corresponds to the pKa of the drug since it is the point at which there is maximum change in absobance with a small change in pH.5 0.6 0 .1 0 5 pH 10 15 303 nm : A b s vs p H 0 .5 0.1 0 -0 .3 ∆Abs/ ∆pHvs pH s b A H p / s b A ∆ 0.4 0 .5 0 .1 0 2 4 6 pH 8 10 12 ∆Abs/∆pHvs pH s b A 0 .A b s vs p H 0 .

.The average of three pka was calculated as: pka = (6 +6+6)/3 pka = 6 CONCLUSION : The pKa of the given drug was found to be 6.

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