Page 1

Page 2

DIAZOTIZATION TITRATION Procaine.HCl, Benzocaine.HCl

ACID-BASE TITRATION Bupivacaine.HCl, Tetrcaine.HCl, Dibucaine, cocaine

NON-AQUEOUS TITRATION Lignocaine HCl, Chlorpromazine, Prilocaine HCl, Oxetacaine

THIN-LAYER CHROMATOGRAPHY Bupivacaine , Procaine.HCl

HPLC Chlorprocaine

Page 3

Weigh accurately about 0.3gWeigh accurately about 0.3g

Dissove in 50ml of 2M HClDissove in 50ml of 2M HCl

Add 3g of KBrAdd 3g of KBr

Cool in ice & Titrate slowly with 0.1M NaNO2

Cool in ice & Titrate slowly with 0.1M NaNO2

End-point determined potentiometrically

End-point determined potentiometrically

Each ml of 0.1M NaNO2 = 0.02728 of C13H20N2O2 Each ml of 0.1M NaNO2 = 0.02728 of C13H20N2O2

Page 4

Weigh accurately about 0.4gWeigh accurately about 0.4g

Dissolve in a mixture of 25ml of HCl & 50ml of water

Dissolve in a mixture of 25ml of HCl & 50ml of water

Cool to 10oC Cool to 10oC

Determine by the nitrite titrationDetermine by the nitrite titration

Each ml of 0.1M NaNO2 = 0.01652g of C9H11NO2Each ml of 0.1M NaNO2 = 0.01652g of C9H11NO2

Page 5

Weigh accurately about 0.25gWeigh accurately about 0.25g

Dissove in a mixture of 5ml of 0.01M HCl & 50ml of 95%ethanol

Dissove in a mixture of 5ml of 0.01M HCl & 50ml of 95%ethanol

Titrate with 0.01M ethanolic sodium hydroxideTitrate with 0.01M ethanolic sodium hydroxide

Determine the end-point potentiometricallyDetermine the end-point potentiometrically

Each ml of 0.01M NaOH = 0.03249g of C18H28N2O HCl Each ml of 0.01M NaOH = 0.03249g of C18H28N2O HCl

Page 6

Weigh accurately about 0.25gWeigh accurately about 0.25g

Dissove in a mixture of 5ml of 0.01M HCl & 50ml of alcoholDissove in a mixture of 5ml of 0.01M HCl & 50ml of alcohol

Titrate with 0.1M ethanolic sodium hydroxideTitrate with 0.1M ethanolic sodium hydroxide

Determine the end-point potentiometricallyDetermine the end-point potentiometrically

Each ml of 0.1M NaOH = 0.03008g of C15H25N2O2 HCl Each ml of 0.1M NaOH = 0.03008g of C15H25N2O2 HCl

Page 7

Dissove 0.3g in a mixture of 15ml 0.01M HCl & 50ml of alcohol

Carry out the potentiometric titration using 0.1M NaOH

Read the volume added between the two points of inflection

1ml of 0.1M NaOH = 37.99mg of C20H30N3O2cl

Dissove 0.25g in a mixture of 5ml of 0.01M HCl & 50ml of alcohol

Carry out the potentiometric titration using 0.1M NaOH

Read the volume added between the two points of inflection

1ml of 0.1M NaOH = 33.98 mg of C17H22NO4cl

Page 8

Weigh accurately about 0.5gWeigh accurately about 0.5g

Dissolve in 30ml of anhydrous glacial acetic acidDissolve in 30ml of anhydrous glacial acetic acid

Add 6ml of mercuric acetate solutionAdd 6ml of mercuric acetate solution

Titrate with 0.1M perchloric acid using crystalviolet indicator

Titrate with 0.1M perchloric acid using crystalviolet indicator

Carry out the blank titrationCarry out the blank titration

Each ml of 0.1M HClO4 = 0.02708g of C14H22N2O HClEach ml of 0.1M HClO4 = 0.02708g of C14H22N2O HCl

Page 9

Weigh accurately about 0.6gWeigh accurately about 0.6g Dissolve in 200ml of acetoneDissolve in 200ml of acetone

Add 15ml of mercuric acetate solutionAdd 15ml of mercuric acetate solution

Titrate with 0.1M perchloric acid using saturated solution of methyl orange

in acetone as indicator

Titrate with 0.1M perchloric acid using saturated solution of methyl orange

in acetone as indicator

Carry out the blank titration Carry out the blank titration

Each ml of 0.1M HClO4 = 0.03553g of C17H19N2S HClEach ml of 0.1M HClO4 = 0.03553g of C17H19N2S HCl

Page 10

Weigh accurately about 0.4g

Dissolve in 20ml of anhydrous glacial acetic acid

Titrate with 0.1M perchloric acid

Determine end-point potentiometrically

Each ml of 0.1M HClO4 = 0.02708g of C14H22N2O HCl

Weigh accurately about 0.4g

Dissolve in 20ml of anhydrous glacial acetic acid

Titrate with 0.1M perchloric acid

Determine end-point potentiometrically

Each ml of 0.1M HClO4 = 0.02708g of C14H22N2O HCl

Weigh accurately about 1g

Dissolve in 50ml of anhydrous glacial acetic acid

Titrate with 0.1M perchloric acid

Determine the end-point potentiometrically

Each ml of 0.1M HClO4 = 0.04676g of C28H41N3O3 HCl

Weigh accurately about 1g

Dissolve in 50ml of anhydrous glacial acetic acid

Titrate with 0.1M perchloric acid

Determine the end-point potentiometrically

Each ml of 0.1M HClO4 = 0.04676g of C28H41N3O3 HCl

Page 11

Test solution : a) Dissolve 0.5g of the substance under examination in 100ml of methanol

b) Dissolve 100ml of the test solution a) to 100ml of methanol

a) Dissolve 0.5g of the substance under examination in 100ml of methanol

b) Dissolve 100ml of the test solution a) to 100ml of methanol

Reference solution :

a) Dilute 5ml of test solution b) to 100ml methanol

b) A 0.5% w/v solution of bupivacaine HCl RS in methanol

a) Dilute 5ml of test solution b) to 100ml methanol

b) A 0.5% w/v solution of bupivacaine HCl RS in methanol

Page 12

Mobile phase : A mixture of 100 volumes of methanol and 0.1 volume of strong ammonium solution

A mixture of 100 volumes of methanol and 0.1 volume of strong ammonium solution

Apply 10µl of each solution to the plate coated with silica gelApply 10µl of each solution to the plate coated with silica gel

After development dry the plate in air and spray with dilute potassium iodobismuthate solution

After development dry the plate in air and spray with dilute potassium iodobismuthate solution

Any secondary spot in the chromatogram obtained with test solution (a) is more intense than the spot in the chromatogram obtained with reference solution(a)

Any secondary spot in the chromatogram obtained with test solution (a) is more intense than the spot in the chromatogram obtained with reference solution(a)

Procedure :

Page 13

Sample: Blood / plasma / biofluids

Column: 150 × 4.6mm / bonded-phase C18

Flowrate: 1ml/min

Injection volume: 50µl

Detector: Uv-210nm

Retention time: 4min

Runtime: 10min

Internal standard: lignocaine

Sample: Blood / plasma / biofluids

Column: 150 × 4.6mm / bonded-phase C18

Flowrate: 1ml/min

Injection volume: 50µl

Detector: Uv-210nm

Retention time: 4min

Runtime: 10min

Internal standard: lignocaine

Page 14

INDIAN PHARMACOEPIA 2007

BRITISH PHARMACOEPIA 2009