Saturday, February 2, 2013

Assay Method (D)





Assay Method of  
Desloratadine Tablet

Sample 
Dissolve powdered sample equivalent to 50 mg Desloratadine in previously neutralized 60 ml glacial acetic acid, using crystal violet solution as indicator. Titrate with 0.1 M perchloric acid and determine the end point.Each ml of 0.1M perchloric acid VS is equivalent to 15.525 mg of Desloratadine.

% of content =   V x F x 15.525 x 100 / W


Assay Method of   
Dexamethason Sodium Phosphate Injection

Mobile Phase
Dissolve 680.5 mg Potassium dihydrogen phosphate (monobasic potassium phosphate) in a mixture of methanol water (1:1) and dilute to 500 ml (0.01 M), filter through a 0.45-micron membrane filter and degas.
Standard 
Dissolve 25 mg of Dexamethasone sodium phosphate in 25 ml of mobile phase, dilute 2 ml to 25 ml with same solvent. Mix and filter this solution with 0.45 m membrane filter before injection.
Sample 
Dilute 5 ml of sample (equivalent to 25 mg Dexamethasone sodium phosphate) to 25 ml with mobile phase, dilute 2 ml of this solution to 25 ml with same solvent. Mix and filter this solution with 0.45 m membrane filter before injection.
Condition
C 18 Column 4.0 x 300 mm / 1.6 ml/ minute / UV at 254 nm


Assay Method of   
Dexamethason Sodium Phosphate Tablet

Mobile Phase
Mixture of methanol and water  at a ratio  70 : 30
Standard 
Dissolve 50 mg of Dexamethasone WS in a 50 ml volumetric flask. Add 25 ml of methanol. Shake for 20 minutes and add sufficient methanol to produce 50 ml. Transfer 5 ml of this solution in a 50 ml volumetric flask and dilute to volume with methanol. Mix and filter this solution with 0.45 µ membrane filter before injection.
Sample 
Take powdered sample equivalent to about 5 mg of Dexamethasone in a 50 ml volumetric flask. Add 25 ml of methanol. Shake for 20 minutes and add sufficient methanol to produce 50 ml. Mix and filter this solution with 0.45 µ membrane filter before injection.
Condition
C 18 Column 4.6 x 250 mm 10 µm / 1.0 ml/ minute / UV at 238 nm


Assay Method of   
Dexibuprofen Tablet

Buffer
Take 0.64 ml Orthophosphoric Acid (H3PO4)[84%] in 1000 ml distilled water.
Ratio   
Accetonitrile : Buffer º 55 : 45
Standard 
Weigh and transfer about 100 mg working standard of Dexibuprofen in a 100 ml volumetric flask. Add 55 ml of
Accetonitrile and shake for 20 minutes and dilute with 0.01 M Orthophosphoric Acid (H3PO4 up to the mark and mix
well. Filter this solution with 0.45 m   membrane filter before injection.
Sample 
Take the weight of 20 tablets and crush it very finely then take the powder equivalent to 100 mg of Dexibuprofen into a 100 ml volumetric flask add 55 ml of Accetonitrile and Sonicate for 15 minutes then shake for 20 minutes and dilute with 0.01 M Orthophosphoric Acid (H3PO4 up to the mark and mix well. Filter this solution with Whatman Filter paper. & Finally filter this solution with 0.45 m membrane filters before injection.
Condition
3.9 x 30 cm  Analytical Column that contains 10 mm packing L8 / UV at 220 nm / 10 minutes.


Assay Method of  
 Dextromethorphan Hydrobromide Syurp

Sample 
Take 5 ml of syrup equivalent to 10mg of Dextromethorphan Hydrobromide in a 250 ml separating funnel. Basify with 3 ml of 25 % w/v solution of sodium hydroxide. Extract two time each with 40 ml quantities of n- hexane. Extract the combined extracts with successive quantities of 40, 20 and 10 ml of 0.1N Hydrochloric acid. Collect the acid layer in a 100 ml of Volumetric flask and dilute to 100 ml with 0.1N Hydrochloric acid. Measure the absorbance of the resulting solution at the maximum at 278 nm .Calculate content of  Dextromethorphan Hydrobromide  taking 70 as the value of A (1% , 1cm ) at the maximum at 278 nm .
% of Dextromethorphan HBr  =         Absorbance   x 100 / Conc. in gm per 100 ml x 70


Assay Method of   
Diazepam Tablet

Sample 
Take powdered sample equivalent to about 10 mg of Diazepam in a 100ml volumetric flask. Add 5 ml of water, mix and allow to stand for 15 minutes. Add 70ml of a 0.5% w/v solution of sulphuric acid in methanol and shake for 15 minutes. Add sufficient methanolic sulphuric acid to produce 100ml. Mix and  filter. Take 10 ml of the filtrate in a 50ml volumetric flask. Make the volume up to the mark with same solvent and measure the absorbance of the resulting solution at the maximum at 284 nm. Calculate the content of Diazepam taking 450 as the valu of A (1%, 1 cm) at 284 nm.
Calculation
 % of Diazepam =  Absorbance of Sample ´ 100 / Conc. Of spl. ´ 450                                      


Assay Method of   
Diazepam Injection


Sample 
To a volume containing 10 mg of Diazepam add 20 ml of mixed phosphate buffer pH 7.0 and extract with four 20-ml quantities of chloroform, passing each extract through the same 5 g of anhydrous sodium sulphate. Combine the chloroform extracts, dilute to 100 ml with chloroform and mix. Evaporate 10 ml to dryness in a current of nitrogen, dissolve the residue in 25 ml of 0.05m methanolic sulphuric acid, mix and measure the absorbance of the resulting solution at the maximum at 368 nm. Calculate the content of Diazepam taking 151 as the value of A(1%, 1 cm) at the maximum at 368 nm.
Calculation
 % of Diazepam =  Absorbance of Sample ´ 100 / Conc. Of spl. ´ 151                                      


Assay Method of   
Diclofenac Sodium Tablet & Suppository

Sample 
Weigh 10 Suppositories & cut into small pieces. Dissolve a quantity containing 100 mg of Diclofenac Na in 60 ml of hot Glacial acetic acid, which is previously neutralized to 1 drop of 0.5 % w/v crystal violet solution by titrating with 0.1 N Perchloric acids. Cool the solution. Titrate Potentiometrically with 0.1 N Perchloric Acid VS. Each ml of 0.1 N Perchloric Acid VSº31.81 mg of Diclofenac Na


Assay Method of  
 Diclofenac Sodium Injection


Sample 
To a volume of sample containing 37.5 mg of Diclofenac Sodium (1 ml) add water to make volume 50ml. Dilute 1 ml to 50 ml with methanol. Measure the absorbance of the resulting solution at 282 nm taking 430 as the value of A (1%, 1 cm).
Calculation
 % of Diclofenac Sodium =  Absorbance of Sample ´ 100 / Conc. Of spl. ´ 430                                      

Assay Method of   
Digoxin Tablet


Standard 
Weigh accurately 5 mg of Digoxin, a Working Standard and transfer it into a 25 ml volumetric flask. Then weigh accurately 10 mg of Spectracol quinoline yellow LK (OEC0014) colour and transfer it into that 25 ml volumetric flask and add approximately 20ml of methanol and shake for 20 minutes to dissolve completely.  Then adjust the volume up to the mark (25ml) with methanol and mix well. Filter the solution by whatman filter paper at least 3 times. Then   Take 3 ml of this solution in another 25 ml volumetric flask and make the volume up to the mark (25 ml) with methanol & mix well . Measure the absorbance of standard solution at wavelength 218 nm using methanol as a blank.
Sample 
Take the average weight of 30 tablets and crush them into fine powder. Transfer 2000 mg powder sample equivalent to 5 mg of Digoxin into a 25 ml volumetric flask. Then add 20 ml of methanol and shake for 5 minutes after that sonicate the solution for 20 minutes to dissolve it completely. Then adjust the volume up to the mark (25 ml) with methanol and mix well. Filter the solution by Whatman filter paper at least 2 times. Then take 3 ml of this filtrate in another 25 ml volumetric flask and make the volume up to the mark (25 ml) with methanol & mix well. Measure the absorbance of sample solution at wavelength 218 nm using methanol as a blank.


Assay Method of   
Digoxin Solution


Buffer
Dissolve 6.805 gm of Potassium dihydrogen orthophosphate with 950 ml  distilled water into 1000 ml volumetric flask, adjust the pH 4.5 ± 0.05 with Phosphoric acid  & make volume with distilled water up to 1000  ml
Ratio   
Phosphate Buffer pH 4.5 ( 70 % ) : Acetonitrile ( 30 % )
Standard 
Accurately weigh and transfer about 10.4 mg of working standard of Digoxin into 50 ml volumetric flask. Add 30 ml of Methanol ( HPLC grade ) & shake for 20 minutes and dilute with Methanol ( HPLC grade ) up to the mark and then sonicate this solution for 10  minutes.Take 6 ml of the solution in a 50 ml volumetric flask. Make the volume up  to mark ( 50 ml ) with Methanol ( HPLC grade ). Filter this solution with 0.45 m membrane filter before injection.
Sample 
Accurately take 25 ml  of Centoxin Solution into 50 ml volumetric flask. Add 10 ml of Methanol ( HPLC grade ) & shake for 20 minutes and dilute with Methanol ( HPLC grade ) up to the mark.Filter this solution with whatman filter paper & finally filter this solution with 0.45 m membrane filter before injection
Condition
ODS1  , 10 m 4.6 x 250 mm / 300 C/ UV at 218 nm/25 minutes


Assay Method of  
 Diosmin & Hespiridin Tablet


Mobile Phase   
Mix 2 volume of Acetonitrile, 6 volume of Glacial Acetic Acid & 28 volume of Methanol with 66 volume of distilled water and then filter through a 0.45-micron membrane filter and degas.
Standard 
For Diosmin:
Dissolve about 22.5 mg of Diosmin WS in 15 ml of Dimethyl Sulfoxide and dilute to 25 ml with the same solvent. Filter this solution with 0.45 m membrane filter before injection.
For Hesperidine:
Dissolve about 10 mg of Heperidine in 60 ml of Dimethyl Sulfoxide and dilute to 100 ml with the same solvent. Filter this solution with 0.45 m membrane filter before injection.
Sample 
Shake a quantity of the powdered sample containing about 22.5 mg of Diosmin & 2.5 mg of Heperidine in 15 ml of Dimethyl Sulfoxide for 30 minutes, dilute to 25 ml with the same solvent and then filter. Filter this solution again with 0.45 m membrane filter before injection.
Condition
C18 Column (4.6 mmx 25cm) & 5µm (ODS1)/ 400 C/ UV at 275 nm


Assay Method of  
 Dipyridamole Tablet

Standard 
Dissolve 50mg Dipyridamole WS in 1M hydrochloric acid and dilute to 100ml. Dilute 1ml to 50ml with 1M hydrochloric acid.Measure the absorbance of both sample & standard solution at 283 nm using 1M hydrochloric acid as blank.
Sample 
Take powdered sample equivalent to about 250 mg of Dipyridamole in a 500ml volumetric flask. Add 300ml of 1M hydrochloric acid, heat at 40°C for 20minutes with shaking, allow to cool and Add 1M hydrochloric acid to make volume 500ml. Filter the solution. Dilute 1ml of the filtrate to 50ml with 1M hydrochloric acid.


Assay Method of
               Diphenhydramine HCl  Tablet  & Syrup

Bromocresol Green Solution
Take 100 mg of Bromocresol green powder into a 100 ml volumetric flask. Add 1.4 ml of 0.1 M NaOH into it. Make the volume up to the mark with pH 5.3 Phosphate buffer.
Phosphate Buffer pH 5.3
Dissolve 27.22 gm of monobasic potassium phosphate (KH2PO4) in 1000 ml of water.

Standard 
                                    Take 25 mg of Diphenhydramine HCl, working standard into a 250 ml volumetric flask. Add 150 ml of water & shake for 10 minutes to dissolve. Make the volume up to the mark with water. Take 5 ml of this solution into a separating funnel. Add 20 ml Phosphate buffer pH 5.3, 5 ml bromocresol green solution & 20 ml chloroform into the separating funnel & proceed the extraction process  by shaking the separating funnel for 10 minutes.When the layer have separated completely, collect the lower layer & repeat the upper layer with two quantities of 10 ml chloroform then collect the lower layer by filtering with whatman filter paper into a 50 ml volumetric flask. Make the volume up to the mark with chloroform. Measure the absorbance of the standard & sample solution at 414 nm taking Chloroform as a blank.
Sample 
Weigh accurately 20 tablets and crush them into fine powder. Take the powdered sample equivalent to 25 mg
of Diphenhydramine HCl, into a 250 ml volumetric flask. Add 150 ml of water into it & shake for 15 minutes.
Make the volume up to the mark with water. Filter the solution with whatman filter paper. Take 5 ml of filtrate
solution into a separating funnel. Add 20 ml Phosphate buffer pH 5.3, 5 ml bromocresol green solution & 20 ml
chloroform into the separating funnel & proceed the extraction process  by shaking the separating funnel for 10
minutes When the layer have separated completely, correct the lower layer & repeat the upper layer with two
quantities of 10 ml chloroform then collect the bottom layer by filtering with whatman filter paper into a 50 ml
volumetric flask. Make the volume up to the mark with chloroform. Measure the absorbance of the standard &
sample solution at 414 nm taking Chloroform as a blank.


Assay Method of   
Domperidone Tablet & Solution
HPLC Method:
Mobile Phase   
0.5% w/v of ammouium acetate  :  Methanol      (50 : 50)

Standard 

Dissolve 10.0 mg of Domperidone to 100.0ml with methanol.
Sample 
Dissolve 10mg Domperidone  (10ml  suspension) in methanol by shaking for 20 minutes , volume to 100ml with methanol and filter through  a glass micro-filter ( Whatman GF/C is suitable ).
Condition
C-8 5µm Column / 280 nm / 1.5ml per minute / 10µl / 3.5min



UV method:
Diluent: Methanol
Dilution: As same as above.
Wavelength: 280nm.

Assay Method of  
 Domperidone Suppository

Sample 
Weigh 10 Suppositories & cut into small pieces. Dissolve a quantity containing 120 mg of Domperidone in 60 ml of Glacial acetic acid, which is previously neutralized to 0.2 ml of Neptholbezein solution by titrating with 0.1 N Perchloric acids. Cool the solution. Titrate Potentiometrically with 0.1 N Perchloric Acid VS. Each ml of 0.1 N Perchloric Acid VSº42.59 mg of Domperidone


Assay Method of   
Doxycycline Hydrochloride Capsule (i)


Standard
Take 57.710 mg of Doxycycline Hydrochloride (Equivalent to 50 mg Doxycycline) working standard in a 50 ml volumetric flask. Add 70 ml of methanol. Shake for 15 minutes. Add methanol to make volume 100 ml. Take 2 ml of the solution in a 100 ml volumetric flask. Make the volume up to mark (100 ml) with methanol. Measure the absorbance at 349 nm taking methanol as blank.
Sample
Take the weight of 20 capsules & determine the average content weight. Crush the total content weight into powder. Take a quantity of the powder containing equivalent to 50 mg of Doxycycline in a 100 ml volumetric flask. Add 70 ml of methanol. Shake for 15 minutes. Add methanol to make volume 100 ml. Filter the solution. Take 2 ml of filtered solution in a 100 ml volumetric flask. Make the volume up to mark (100 ml) with methanol. Measure the absorbance at 349 nm taking methanol as blank.


Assay Method of   
Doxycycline Hydrochloride Capsule (ii)

Standard
Prepare standard in the same way .as sample preparation .Conc. 0.001 % Doxycycline  WS in  0.1N Hydrochloric acid  .Measure the absorbance at 271 nm , taking  0.1N Hydrochloric acid  as Blank .
Sample
Weigh and powder 20 capsules. Take powder  equivalent to  50 mg of Doxycycline in 100 ml volumetric flask. Add 60 ml of 0.1N Hydrochloric acid  and shake for 20 minutes. Make the volume up to 100 ml with the same solvent . Mix and filter. Dilute 1 ml of the filtrate to 50 ml with  0.1N Hydrochloric acid .


Assay Method of   
Drotaverine Hydrochloride Tablet

Sample 
Dissolve powdered sample equivalent to 100 mg Drotaverine Hydrochloride in previously neutralized mixture of 60 ml glacial acetic acid and 5% Mercury (II) Acetate (50 ml + 10 ml) using crystal violet solution as indicator. Titrate with 0.1 M Perchloric acid and determine the end point.Each ml of 0.1M perchloric acid VS is equivalent to 43.39 mg of Drotaverine Hydrochloride.

% of content = V x F x 43.39 x 100 / W


Assay Method of   
Drotaverine Hydrochloride Injection ( Method – 01 )


Sample 
Dilute sample equivalent to 200 mg of Drotaverine HCl with 50 ml of water. Acidify  with 2 M nitric acid . Titrate with 0.1M silver nitrate , determining the end –point potentiometrically using a silver indicator electrode and a silver-silver chloride reference electrode.  (Electrode DM –141 , Instrument Mettler DL 40 RC Memotitrator )
1 ml of 0.1M silver nitrate is equivalent to 43.39 mg of  Drotaverine hydrochloride

% of Drotaverine HCl: No. of ml of 0.1M silver nitrite VS x F x 43.39 x 100 / Amount of sample in mg


Assay Method of  
 Drotaverine Hydrochloride Injection ( Method – 02 )

Sample 
Take sample equivalent to 100 mg of Drotaverine Hydrochloride in a conical flask. Add 5 ml of 2M Nitric acid  and 5 ml of 0.1 M silver nitrate VS . Shake for 5 minutes. Add 2 ml of Nitrobenzene and shake for another 5 minutes. Add 2 ml of 10% ferric ammonium sulphate Solution as indicator and titrate the excess silver nitrate with 0.1 M ammonium thiocyanate VS. To the end point a Blood-red colour appears. 
1 ml of  .1 M silver nitrate VS @ 43.39 mg of Drotaverine Hydrochloride.
Calculation
(V1 x S1 – V2 x S2 ) x 43.39 x100 / Amount of Drotaverine Hydrochloride




3 comments:

  1. Plese tell me the assay procedure for Diethylamine Salicylate.

    ReplyDelete
  2. Please tell me the uv method for cefixime and ofloxacin combination in tablets as well as cefixime with ornidazole

    ReplyDelete