BUSPIRONE HYDROCHLORIDE USP



BUSPIRONE HYDROCHLORIDE USP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Buspirone Hydrochloride USP from the Pharmacopoeial specifications.
2.0  SCOPE:
This SOP shall be applicable in Q.C laboratory.
3.0  RESPONSIBILITY:
3.1  Q.C Analyst.
4.0  ACCOUNTABILITY:
4.1  Q.C Manager.
5.0  PROCEDURE:
5.1  Identification tests:
5.1.1        Chlorides test:
5.1.1.1  Material and equipment:
5.1.1.1.1        Glassware (according to requirement).
5.1.1.1.2        Analytical weighing balance.
5.1.1.1.3        Centrifuge machine.
5.1.1.1.4        Dilute nitric acid.
5.1.1.1.5        0.5ml of Silver nitrate TS.
5.1.1.1.6        Nitric acid solution.
5.1.1.1.7        Ammonia.
5.1.1.1.8         Purified water.
5.1.1.2  Sample:
5.1.1.2.1        10.0mg/ml in purified water.
5.1.1.3  Method:
5.1.1.3.1        Take a test tube add in it 10.0mg/ml in purified water of test solution with the help of pipette.
5.1.1.3.2        Add one drop of diluted nitric acid and 0.5ml of silver nitrate TS to a solution of the substance being examined containing.
5.1.1.3.3        Centrifuge the mixture without delay, in centrifugation machine,
5.1.1.3.4        And decant the supernatant layer.
5.1.1.3.5        The obtained ppt is wash with three 1ml, of portions of nitric acid solution (1 in 100).
5.1.1.3.6        And discard the washing.
5.1.1.3.7        Add ammonia TS dropwise to this precipitate.
5.1.1.3.8        Observe the changes.
5.1.1.4  Observations:
5.1.1.4.1        It dissolves readily.
5.2  Assay:
5.2.1        Apparatus:
5.2.1.1  Glassware (according to requirement).
5.2.1.2  Magnetic stirrer.
5.2.1.3  HPLC apparatus.
5.2.1.4  Analytical weighing balance.
5.2.1.5  Monobasic potassium phosphate.
5.2.1.6  Sodium hydroxide.
5.2.1.7  Acetonitrile.
5.2.1.8  Propylparaben.
5.2.1.9  Methanol.
5.2.1.10 1N hydrochloric acid.
5.2.1.11 Purified water.
5.2.2        Buffer:
5.2.2.1  Prepare 1.36 mg/ml of monobasic potassium phosphate in water.
5.2.2.2  Adjust the solution with 10% sodium hydroxide (w/v) to a pH of 7.5.
5.2.2.3  And then filter it by using filtration apparatus.
5.2.3        Mobile phase:
5.2.3.1  Prepare mobile phase Acetonitrile and Buffer (2:3) according to the need.
5.2.4        Internal standard stock solution:
5.2.4.1  Prepare internal standard stock solution 2.5mg/ml of propylparaben in methanol.
5.2.5        Internal standard solution:
5.2.5.1  Prepare internal standard solution 0.125mg/ml of propylparaben from the internal standard stock solution in purified water.
5.2.6        Standard stock solution:
5.2.6.1  Take a 100.0ml of volumetric flask and add 50.0mg of USP Buspirone Hydrochloride RS.
5.2.6.2  Dissolve it in 25.0ml of 1N hydrochloric acid by using magnetic stirrer.
5.2.6.3  Dilute it with purified water up to the volume.
5.2.7        Standard solution:
5.2.7.1  Take a 50.0ml of volumetric flask and add 10.0 ml of standard stock solution and 10.0 ml of internal standard solution in it.
5.2.7.2  Dilute it with purified water up to the volume.
5.2.8        Sample stock solution:
5.2.8.1  Take a 100.0ml of volumetric flask and add 50.0mg of buspirone hydrochloride in it.
5.2.8.2  Add 25.0ml of 1N hydrochloric acid. Dissolve it by using magnetic stirrer
5.2.8.3  Dilute it with purified water up to the volume.
5.2.9        Sample solution:
5.2.9.1  Prepare 0.1mg/ml of buspirone hydrochloride from the sample stock solution and 0.025mg/ml of propylparaben from the internal standard solution in purified water.
5.3  Chromatographic system:
5.3.1        Mode: Liquid chromatography.
5.3.2        Detector: UV 254 nm.
5.3.3        Column: 3.9-mm × 30-cm; packing L1.
5.3.4        Flow rate: 2.0mL/min.
5.3.5        Injection size: 25μL.
5.4  System suitability:
5.4.1        Samples: Standard solution.
[NOTE-----The relative retention times for propylparaben and buspirone hydrochloride are 0.55 and 1.0, respectively.]
5.4.2        Suitability requirements:
5.4.2.1  Resolution: NLT 4 between buspirone hydrochloride and the internal standard.
5.4.2.2  Relative standard deviation: NMT 2.0%.
5.5  Analysis:
5.5.1        Samples: Standard solution and sample solution.
5.5.2        Calculate the percentage of buspirone hydrochloride (C21H31N5O2.HCl) in the portion of buspirone hydrochloride taken:
Result = (RU/RS) x (CS/CU) x 100
RU = peak response ratio of Buspirone hydrochloride to propylparaben from the sample solution.
RS = peak response ratio of Buspirone hydrochloride to propylparaben from the standard solution.
CS = concentration of USP Buspirone Hydrochloride RS in the standard solution (mg/ml).
CU = nominal concentration of Buspirone Hydrochloride in the standard solution (mg/ml).
5.6  Procedure:
5.6.1        Equilibrate the column and detector with mobile phase at specified flow rate until a constant signal is received.
5.6.2        Separately inject equal volumes about 25μL of the standard solution and sample solution.
5.6.3        Record the chromatogram.
5.6.4        Measure the responses for the major peaks.
5.6.5        Analyze as directed in the monograph.
5.7  Limit:
5.7.1        97.5%-102.5%.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  USP38NF33 Volume-3 Official Monograph/ Buspirone Hydrochloride: 2015, pp.: 2495-2496.
7.2  The British Pharmacopoeia. Vol V., Official Monograph /Qualitative Reactions and Tests: 2015, pp. 266-270.
8.0  ANNEXURES:
Annexure 1: Observations and calculations of HPLC method







Annexure: 1
Observations and calculations of HPLC method
Analysis on HPLC
Instrument: ___________________                                           Date: _________________
Model: ___________________           
Column size:
Length=
θ=
Stationary phase:

Temperature:

Mobile phase:

Flow rate:

Injection size:

Detector:

Wavelength:
λ=

Sample solution: _______________________
Reference standard solution: ______________
Impurities: ____________________________
(calculate each component calculation separately)
OBSERVATIONS:
Attach spectrum.






CALCULATIONS:
1.      Retention time:                                                                                n= no. of peak
Retention time of unretained peak (tm)= _____________
No. of peaks
Retention time of peak of interest
(tr)n
Height of peak of interest
(h)n
Width of peak of interest
(w)n
Area of peak of interest
A=1/2(h x w)




















2.      Retention volume:
Flow rate= _______________ml/min.
No. of peaks
Retention time of peak of interest
(tr)n
Retention volume = retention time x flow rate












3.      Retention factor:
Retention time of unretained peak (tm)= _____________
No. of peaks
Retention time of peak of interest
(tr)n
Retention factor of a component
k= (tr-tm)/tm













4.      Separation factor (α):
No. of peaks
Retention factor of a component
(kn)
Relative retention of two adjacent peaks
α = k2/k1












5.      Resolution:
Retention time of unretained peak (tm)= _____________
No. of peaks
Retention time of peak of interest
(tr)n
Width of peak of interest
(w)n
Resolution
Rs = 2 (tr2-tr1)
        (w1-w2)
















6.      Efficiency:
No. of peaks or components
Retention time of peak of interest
(tr)n
Width of peak of interest
(w)n
Efficiency
(No. of theoretical plates)
N= 16 (tr/w)2


















7.      Height equivalent to a theoretical plate (HETP):
Length of column = ________________________
No. of peaks or components
No. of theoretical plates
(N)
Height equivalent to a theoretical plate HETP = L/N












8.      Symmetry factor (tailing factor):
No. of peaks or components
Distance from the peak max. to leading edge of the peak
(f)
Width w
Symmetry factor
At 5%
At 10%
As = w5%
       2f
As = w10%
       2f
























9.      Response factor & Relative response factor:
Conc. (mg/ml)= ___________________
No. of peak
Peak area
Response factor = (peak area/conc.)
Relative response factor = (response factor of impurity/response factor of API)

















10.  Relative standard deviation (%RSD):
Use formula of relative standard deviation where it is required i.e.,


11.  Percentage of content:
Percentage content = (rU/rS) x (CS/CU) x 100.
rU= peak response of substance from the sample solution.
rS= peak response of substance from the standard solution.
CS= concentration of substance in the standard solution (mg/mL).
CU= concentration of substance in the sample solution (mg/mL).









RESULTS:
________________________________________________________________________________________________________________________________________________


9.0  ABBREVIATIONS:
Abbreviation
Expanded Form
SOP
Standard operating procedure
&
And
No.
Number  
Ltd.
Limited
QCA
Quality control active ingredient
F
Format
Q.C
Quality control
Vol
Volume
g
Grams
ml
Milliliter
Min
Minutes
oC
Degree centigrade
mg
Milligram
M
Molar
%
Percentage
TS
Test solution
R
Reagent
g/L
Gram per liter
ppt
Precipitates
N
Normal
USP
United states pharmacopoeia
NF
National formulary
cm
Centimeter
nm
Nanometer
mm
Millimeter
Approx.
Approximately
%
Percentage
μL
Microliter
θ
Theta
λ
Lambda
w/v
Weight by volume
mg/ml
Milligram per milliliter
UV
Ultraviolet
ml/min
Milliliter per minute


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