TAMSULOSIN HYDROCHLORIDE USP METHOD OF ANALYSIS SOP


TAMSULOSIN HYDROCHLORIDE USP METHOD OF ANALYSIS SOP


1.0  OBJECTIVE:
To lay down a procedure for the active raw material of the Tamsulosin 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.
5.1.1.2  Sample:
5.1.1.2.1        7.5mg/ml in purified water.
5.1.1.3  Method:
5.1.1.3.1        Take a test tube add in it 7.5mg/ml in purified water, use heat to dissolve the sample.
5.1.1.3.2        Cool 5.0ml of the solution in ice-bath.
5.1.1.3.3        Add 3.0ml of diluted nitric acid by using pipette. Shake it until it mixed thoroughly.
5.1.1.3.4        Allow to stand for 30min at room temperature and filter it by using filtration apparatus.
5.1.1.3.5        Observe the changes.
5.1.1.4  Observations:
5.1.1.4.1        A white curdy ppt is formed.
5.1.2        Specific optical rotation:
5.1.2.1  Material and equipment:
5.1.2.1.1        Polarimeter.
5.1.2.1.2        Analytical weighing balance.
5.1.2.1.3        Magnetic stirrer.
5.1.2.1.4        Glassware (1 beaker of 50.0ml, 1 stirrer, 1 spatula).
5.1.2.1.5        Purified water.
5.1.2.2  Sample:
5.1.2.2.1        7.5mg/ml in purified water.
5.1.2.3  Method:
5.1.2.3.1        Take a beaker and prepare 7.5mg/ml in purified water.
[NOTE: Sample should be previously dried at 105o for 2h; heat at 60o-70o to dissolve, and allow to cool before using.]
5.1.2.3.2        Firstly clean the Polarimeter with clean dry cloth, according to SOP
5.1.2.3.3        Operate the Polarimeter according to SOP
5.1.2.3.4        Fill the Polarimeter tube with blank solution and determine the observed optical rotation.
5.1.2.3.5        Similarly, fill the Polarimeter tube with sample solution and determine the observed optical rotation.
5.1.2.3.6        Note down the values in annexure-1.
5.1.2.3.7        Calculate the specific optical rotation with reference to anhydrous substance by using formula:
                                                      [α]λ T = α/lc
5.1.2.4  Observations:
5.1.2.4.1        -17.5o to -20.5o at 20oC.
5.2  Loss on drying:
5.2.1        Material and equipment:
5.2.1.1  Glassware (according to requirement).
5.2.1.2  Analytical weighing balance.
5.2.1.3  Oven.
5.2.2        Sample:
5.2.2.1  1.0g.
5.2.3        Method:
5.2.3.1  Weigh 1.0g of the test sample.
5.2.3.2  Set the oven apparatus. Operate it according to the SOP
5.2.3.3  Place the sample into the tray and dry it.
5.2.3.4  Set the temperature of oven at 105oC for at least 2h.
5.2.3.5  And wait till the sample loses its moisture.
5.2.3.6  After 2h weigh the sample again by using analytical weighing balance i.e. the final weight.
5.2.3.7  Note down readings on given Annexure-2.
5.2.4        Observation:
5.2.4.1  NMT 0.5%.
5.3  Assay:
5.3.1        Apparatus:
5.3.1.1  Glassware (according to requirement).
5.3.1.2  Magnetic stirrer.
5.3.1.3  Liquid chromatography apparatus (HPLC).
5.3.1.4  Analytical weighing balance.
5.3.1.5  1.0g of octanesulfonic acid sodium salt.
5.3.1.6  1.0ml of phosphoric acid.
5.3.1.7  Acetonitrile.
5.3.1.8  Methanol
5.3.1.9  Purified water.
5.3.2        Buffer:
5.3.2.1  Take a beaker of 1000.0ml and transfer 1.0g of octanesulfonic acid sodium salt and 1.0ml of phosphoric acid.
5.3.2.2  Add sufficient quantity of purified water and dissolve it by using magnetic stirrer i.e. SOP
5.3.2.3  And finally make up the volume up to 1000.0ml.
5.3.3        Mobile phase:
5.3.3.1  Prepare mobile phase Acetonitrile and Buffer (20:80) according to the need.
5.3.4        Diluent:
5.3.4.1  Prepare diluent methanol and purified water (75:25) according to the need.
5.3.5        Standard solution:
5.3.5.1  Take a beaker and add 0.016mg/ml of USP tamsulosin hydrochloride RS in diluent.
5.3.5.2  And mix it thoroughly by using magnetic stirrer i.e. SOP
5.3.6        Sample solution:
5.3.6.1  Take a beaker and add 0.016mg/ml of tamsulosin hydrochloride in diluent.
5.3.6.2  And mix it thoroughly by using magnetic stirrer i.e. SOP
5.3.7        Chromatographic system:
5.3.7.1  Mode: Liquid chromatography.
5.3.7.2  Detector: UV 225nm.
5.3.7.3  Column: 4.6-mm × 15-cm; 3.5μm packing L1.
5.3.7.4  Column temperature: 30o.
5.3.7.5  Flow rate: 1.5mL/min.
5.3.7.6  Injection size: 10μL.
5.3.8        System suitability:
5.3.8.1  Samples: Standard solution.
5.3.8.2  Suitability requirements:
5.3.8.2.1        Relative standard deviation: NMT 0.85% for six replicate injections.
5.3.9        Analysis:
5.3.9.1  Samples: Standard solution and sample solution.
5.3.9.2  Calculate the percentage of tamsulosin hydrochloride (C20H28N2O5S.HCl) in the portion of tamsulosin hydrochloride taken:
Result = (rU/rS) x (CS/CU) x 100
rU= peak response of tamsulosin from the sample solution.
rS= peak response of tamsulosin from the standard solution.
CS= concentration of USP tamsulosin Hydrochloride RS in the standard solution (mg/ml).
CU= concentration of tamsulosin Hydrochloride in the sample solution (mg/ml).
5.4  Procedure:
5.4.1        Equilibrate the column and detector with mobile phase at specified flow rate until a constant signal is received.
5.4.2        Separately inject equal volumes about 10μL of the standard solution and sample solution.
5.4.3        Record the chromatogram.
5.4.4        Measure the responses for the major peaks.
5.4.5        Analyze as directed in the monograph.
5.5  Limit:
5.5.1        98.0%-102.5% on the dried basis.
6.0  REVISION LOG:
Revision No.
Effective Date
Reason
00

New SOP

7.0  REFERENCES:
7.1  USP38NF33 Volume-1 Official Monograph/ Identification test-General: 2015, pp.: 216-219.
7.2  USP38NF33 Volume-6 Official Monograph/ Tamsulosin Hydrochloride: 2015, pp.: 5441-5442.
7.3  USP38NF33 Volume-1 Official Monograph/ Chromatography: 2015, pp.: 424-434.
8.0  ANNEXURES:
Annexure 1: Specific optical rotation observations and calculations.
Annexure 2: Observations of Percentage Loss of drying by using oven.
Annexure 3: Observations and calculations of HPLC method.


Annexure: 1
Specific optical rotation observations and calculations
Specific optical rotation
Instrument: ___________________                                              Date: _______________
Model: _______________________        Length of Polarimeter tube: ________________
Sample: ________________________________g.
Solvent: ________________________________ml.
Concentration of sample solution: ____________g/ml.
Blank solution:
Sr.#
Blank solution
Temperature
Optical rotation
(α)












                                                                                                 Average: _______________
Optical rotation of blank solution: _______________
Sample solution:
Sr.#
Sample solution
Temperature
Optical rotation
(α)












                                                                                                 Average: _______________
Optical rotation of sample solution: ______________
Optical rotation of substance = Blank solution - Sample solution.




Specific optical rotation of sample solution by using formula:
[α]λ T = α/lc




















                                                                      Result: ________________
Remarks: ___________________________________________________________



Annexure: 2
Observations of percentage loss of drying by using Oven
Percentage loss of drying by using Oven
Apparatus: ____________________
Temperature: __________________
Weight of Sample = _____________
Time period = _____________
Pressure= _________________
Sr.#
Time (min)
Weight of sample (g)
% Loss of Moisture
Initial weight
Final weight















Average % Loss of Moisture: _____________

% Loss of Moisture:








Remarks: _______________________________________________________________



Annexure: 3
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 chromatogram.







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
USP
United states pharmacopoeia
NF
National formulary
cm
Centimeter
nm
Nanometer
mm
Millimeter
Approx.
Approximately
%
Percentage
μL
Microliter
θ
Theta
λ
Lambda
mg/ml
Milligram per milliliter
UV
Ultraviolet
ml/min
Milliliter per minute
o
Degree (angle)
l
Length
c
Concentration (g/ml)
g/ml
Gram per milliliter
α
Alpha
T
Temperature


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