Friday, December 10, 2010

FORMAT FOR CALIBRATION RECORD OF HPLC

Annexure – 1    :  Format For Calibration Record Of Pump (Flow Rate)
Annexure – 2    :  Format For Calibration Record Of Gradient Proportionate Valve
Annexure – 3    :  Format For Calibration Record Of Injector
Annexure – 4    :  Format For Calibration Record Of Detector

ANNEXURE – 1

FORMAT FOR CALIBRATION RECORD OF HPLC

REF. SOP NO.:  
Revision No.:  00
Page No.: 1 of 1
Effective from: 




Calibration Record     :           High Performance Liquid Chromatograph
Instrument No.           :
Make And Model       :
Calibration Date         :
Calibration Due On    :

Calibration Of Pump (Flow Rate):

Flow rate adjusted to 1.0 ml / min.
Observed weight in gm.
Limit in ml / min.
1
2
Mean wt. / min
Mean Vol. / min
Pump-A
Weight of beaker + water after 10 min. (W2)




0.99 to 1.01
Weight of beaker (W1)


(W2 – W1) / 10


Pump-B
Weight of beaker + water after 10 min. (W2)




0.99 to 1.01
Weight of beaker (W1)


(W2 – W1) / 10



Weight per ml of water =        ________ gm.



Calibrated By:                                                            Checked By:  
Date                                                                            Date : 


ANNEXURE – 2


FORMAT FOR CALIBRATION RECORD OF HPLC

REF. SOP NO.:  
Revision No.:  00
Page No.: 1 of 1
Effective from:



Calibration Record     :           High Performance Liquid Chromatograph
Instrument No.           :
Make And Model       :
Calibration Date         :
Calibration Due On    :

Calibration Of Gradient Proportionate Valve
Parameters :

Mobile Phase              : Reservoir  A 100% Water with HPLC
Reservoir B 0.3% Acetone HPLC 
Wavelength                 : 254 nm.
Flow rate                     : 2 ml / min.

Tine Range
Height From Base Line To B Concentration Peak.
Value Obtained
Actual Value Set In The Program
0.01 To 10.0

(Lt: 9.9 To 10.1)

10.01 To 20.0

(Lt: 49.5 To 50.5)

20.01 To 30.0

(Lt: 89.1 To 90.9)


Value  :      Height of B Concentration
                             --------------------------------------  
                  Height of a 100 % Concentration              


Remarks:    Satisfactory  / Not Satisfactory


Calibrated By:                                                            Checked By:  
Date                                                                            Date :


ANNEXURE – 3

FORMAT FOR CALIBRATION RECORD OF HPLC

REF. SOP NO.:  
Revision No.:  00
Page No.: 1 of 1
Effective from: 

Calibration Record     :           High Performance Liquid Chromatograph
Instrument No.           :
Make And Model       :
Calibration Date         :
Calibration Due On    :
Calibration Of Injector : 1. Check for Precision:
Standard Preparation:
Take ______ mg of Uracil (about 50 mg) à 250 ml. à 5ml à 50ml with Methanol.
Parameters:
Mobile Phase : Methanol HPLC grade.       Column  :  ODS (150 mm x  4.6 mm. 5 micron)
Wavelength  :  254 nm.      Flow rate :  1 ml / min.    Injection volume : 20 ml.
Inject six replicate injection of standard solution and calculate RSD for area of main peak.
Injection no.
Area
% of RSD
Limit
1


Not More Than 1.0 %
2

3

4

5

6


2.Check for Linearity :
Sr. No.
Injection volume
Area
Mean
Correlation coefficient
Observed results
Limit
1
10 ml.
i) 
ii)


Not less than 0.99
2
20 ml.
i)
ii)


3
30 ml.
i)
ii)


4
40 ml.
i)
ii)


5
50 ml.
i)
ii)


Remarks: Satisfactory / Not satisfactory.

Calibrated By:                                                            Checked By:  
Date                                                                            Date :


ANNEXURE – 4

FORMAT FOR CALIBRATION RECORD OF HPLC

REF. SOP NO.:  
Revision No.:  00
Page No.: 1 of 1
Effective from: 

Calibration Record     :           High Performance Liquid Chromatograph
Instrument Sr. No.                  :
Make And Model       :
Calibration Date         :
Calibration Due On    :

Calibration Of Detector

Standard Preparation:

Take _____ mg of Uracil ( about 50 mg.) à250 ml. à 5ml à 50ml with Methanol.

Parameters:
Mobile Phase:  Methanol HPLC grade       Column:  ODS (150 mm x 4.6 mm. 5 micron)
Wavelength:  252- 264 nm with 2 nm increment.      Flow Rate:  1 ml / min.    Injection Volume: 20 ml.

Sr.No.
Wavelength (nm)
Area
Mean
1
252
1)
2)

2
254
1)
2)

3
256
1)
2)

4
258
1)
2)

5
260
1)
2)

6
262
1)
2)

7
264
1)
2)

Largest peak response is observed at __________ nm. (Limit: 258 nm  ± 2 nm)
Remarks: Satisfactory / Not Satisfactory.

                                 
Calibrated By:                                                            Checked By:  
Date                                                                            Date :

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