qualification of analytical instruments..M pharmacy 1st year.validation

electronic balance
uv-visible spectrophotometer

1. Qualification of analytical instruments: Electronic balance , UV-Visible spectrophotometer Submitted by Pattan Sohail M pharm 1 st year

2. • Validation of an analytical procedure is the process by which it is established, by laboratory studies, that the performance characteristics of the procedure meet the requirements for the intended analytical applications.” (Definition of Validation: USP) • Qualification is part of validation but the individual qualification steps alone do not constitute process validation • Qualification deals with components or elements of a process • Validation deals with the entire manufacturing process of a product

3. QUALIFICATION OF BALANCES “Qualification of Equipment”, which together should be used when planning, performing and documenting the qualification process of balances • The core document contains the introduction and general forms for Level I and II of qualification, which are common to all types of instruments.

4. AIM AND SCOPE OF THE GUIDELINE This guideline describes the requirements for balances (electronic - digital) used in chemical and biological tests in OMCLs. The following types of balances are considered in this guideline Type Ordinary name No.of digits after decimal position(g) Accuracy class 1. Ultra micro balance 7 I 2. Micro balance 6 I 3. Semi-micro balance 5 I 4. Analytical balance 4 I 5. Precision balance 1 TO 3 II 6. Technical balance 0 TO 1 III

5. CONSIDERATIONS FOR LEVEL I AND II OF EQUIPMENT: QUALIFICATION At Level I of the qualification of balances (selection of instruments and suppliers), it is recommended to select a manufacturer of balances that can satisfy the needs of the laboratory and works under ISO 9001 certification. At Level II of the qualification of balances (installation and release for use), it is recommended to check all the requirements set during the selection of the instrument and calibration should be performed before putting into service by an accredited external service supplier, or internally by appropriately qualified personnel, using certified reference weights according to an approved procedure.

6. 4. REQUIREMENTS FOR BALANCE USE Location of the Balance The accuracy and precision of weighing results are closely associated with the location of the balance. OMCLs should ensure that the balance can work under optimal conditions (weighing room/laboratory, weighing bench, temperature, light, air, etc ,.) • It should be ensured that the weighing bench is stable, no matter from what material it is made. The weighing bench should not deform when work is carried out on it and it must be vibration-proof or the transfer of vibrations must not influence the weighing process.

7. Temperature As weighing results are influenced by temperature, OMCLs should ensure a constant temperature is maintained in weighing rooms/laboratories. The deviation should not exceed more than 5 °C per hour. Atmospheric humidity The optimum relative humidity (% RH) during a weighing process is between 40 % to 60 % 80 % in cases where the accuracy and linearity of measurements are not affected. Light Balances should be protected from direct sunlight (heat). Air OMCLs should not place balances in the airflow of air conditioners or devices with ventilators next to doorways or in areas of high traffic.

8. Weighing vessel OMCLs must ensure that: the smallest possible weighing vessels are used. - if the materials that the weighing vessel is made of have a high degree of electrical insulation they are not electrostatically charged.

9. FREQUENCY OF QUALIFICATION OMCLs must ensure that qualification/calibration of balances is done on receipt (i.e. immediately after delivery) or prior to their first use and after any repair or move. The frequency of qualification/calibration depends on the extent of use of the balances and is at the discretion of individual OMCLs. Qualification/calibration must be performed in accordance with a pre-determined protocol in which acceptance criteria are defined • k = correlation coefficient • SD = standard deviation • RSD = relative standard deviation

10. Parameter to be checked Frequency Typical tolerance limit Levelling Every day before weighing begins Acceptance limits of the balance Internal caliberation Every day before weighing begins Automatic acceptance limits of the balanc Verification Atleast once a week OMCLs shall define their own acceptance criteri . Accuracy Frequency to be defined by OMCL,typically once a year OMCLs shall define their own acceptance criteri . Linearity Frequency to be defined by OMCL,typically once a year OMCLs shall define their own acceptance criteri . (k= 1±0.0001) Precission Frequency to be defined by OMCL,typically once a year OMCLs shall define their own acceptance criteri . (SD=max 5*d) Eccentricity Frequency to be defined by OMCL,typically once a year OMCLs shall define their own acceptance criteri . (RSD=0.05%)

11. Verification Verification of the balance is performed by placing a suitable weight in the centre of the weighing pan once and comparing the result with pre-defined acceptance criteria. The same weight should always be used in these verifications. The acceptance criteria shall be defined by each individual OMCL. Accuracy The accuracy of the balance is checked by weighing at least three different certified weights that cover the usual weighing range of the balance. It is recommended that the weights have approximately 5%, 50% and 100% of the maximum capacity of the balance depending on the type of balance. It is recommended that the weighing is repeated at least 5 times for every weight.

12. Linearity The results obtained from a series of accuracy checks can be used to calculate the correlation coefficient and to check for linearity. The correlation coefficient is calculated by comparing the nominal and measured masses of the weights. The acceptance criteria for the correlation coefficient shall be defined by each individual OMCL. Precision The precision of the balance should be verified by weighing at least 5 times a weight that is equivalent to approximately 50% of the maximum capacity of the balance. It is recommended to repeat the test with a weight that is equivalent to approximately 5% of the maximum capacity of the balance, if the balance is used at the lower range (Proposed criterion: SD = max 5*d, where d = (actual) scale interval (e.g. d=0.1 mg ).

13. CALIBRATION OF UV-VISIBLE SPECTROPHOTOMETER Tests Performed In UV-Visible Spectroscopy : Baseline flatness test UV region wave length accuracy test Visible region wave length accuracy test %Transmittance of Cuvette Control of absorbance Emission lines from deuterium discharge lamp Stray Light measurement Resolution power Photometric linearity

14. Make, Soft ware & Version Model type & Serial No Beam type (single/double) INS/ EQP.ID No. SOP No Calibration Frequency Every six months Instrument/Equipment Calibration Record INS/ EQP Name: UV-VISIBLE spectrophotometer Department Name: Central Instrumentation Lab Equipment Details:

15. Baseline Flatness Test: Measurement configuration parameters : Reference : No Cuvette Sample : No Cuvette Cuvette material : Quartz Wave length range : 200-800 Lamp : Deuterium lamp Detector : PDA detector

16. WAVE LENGTH MEASURED ABSORBANCE ACCEPTANCE CRITERIA 200 ±0.001 300 ±0.001 400 ±0.001 500 ±0.001 600 ±0.001 700 ±0.001 800 ±0.001

17. 2) Uv Region Wave Length Accuracy Test: Measurement configuration Parameters Reference : Air (Empty Cuvette) Sample : Benzene Recording range : 220-270nm Lamp : Deuterium Discharge Detector : PDA Detector WAVE LENGTH (nm) OBSERVED PEAKS AT WAVE LENGTH (nm) ACCEPTANCE CRITERIA 220-270 nm 235.9±0.5nm

18. 3) Visible Region Wave Length Accuracy Test: Measurement Parameters: Reference : Distilled Water Sample : 0.01 % KMno4 Measuring mode : 300 to 600nm Lamp : Deuterium Discharge Detector : PDA Detector WAVE LENGTH (nm) OBSERVED PEAKS AT WAVE LENGTH(nm) ACCEPTANCE CRITERIA 300-600nm 310±1nm 525±1nm

19. 4) %Transmittance Of Cuvette: Measurement configuration Parameters Reference : Empty Cuvette Sample : Empty Cuvette Cuvette material : Quartz Measuring mode : 240nm Lamp : Deuterium discharge lamp Detector : PDADetector WAVE LENGTH(nm) %TRANSMITTANCE ACCEPTANCE CRITERIA 240nm Not less then 80%

20. 5) Control of absorbance: Absorbance:Visible region Place dummy Cuvette in sample holder and set %T to “zero”. Now remove dummy Cuvette, by using fine & coarse control set a reading exactly 40.0 on the read out.  Press Absorbance push button. If the maximum absorbance obtained at λ of 485nm is 0.398 ± 0.002, the photometric calibration of instrument is confirmed to be proper. To confirm, repeat above steps, and set 10.00 on read out Press Absorbance button. If the λ at 485 nm is 1.000±0.002 then it is confirmed the photometric performance in the visible region is proper. Absorbance:U.V region Place blank0.1N H2SO4 Cuvette and 60ppm K2Cr2O7 as sample Set λ exactly to 257 nm, if the value of Absorbance of sample at the set λ is 0.864±0.005, the instrument is measuringAbsorbance properly.

21. 6) Emission Lines From Deuterium Discharge Lamp: Measurement configuration Parameters: Reference : No Cuvette Sample : Empty Cuvette Recording range : 400-500, 600-700 THEORETICAL VALUE OBSERVED VALUE DIFFERENCE ACCEPTANCE CRITERIA 486nm 486±0.3nm 656nm 656 ±0.3nm

22. 7) Stray Light measurement: Weigh accurately 1.2g of dried Potassium chloride in 100 ml volumetric flask and makeup to mark with Double distilled water. Measure the absorbance at 200 nm. Acceptance criteria: Tolerance limit NLT 2.0 8)Resolution Power : Prepare 0.02%v/v solution of Toluene and make up with Hexane. Scan the wavelength from 250 to 280nm. Maximum absorbance is 269 nm and Minimum absorbance is 266nm Acceptance criteria: Ratio limit NLT 1.5

23. 9) Photometric linearity: Weigh accurately 100mg of Potassium chromate in 100ml volumetric flask and dissolve in 0.05N Potassium hydroxide solution. Make up with the same solvent. From the above solution take 20ml and make up to 500ml with 0.05N Potassium hydroxide solution. Now prepare dilution of 4,8,16,24,32 µg/ml. Measure the absorbance at 370nm using blank. Acceptance criteria: The plot should be linear and regression coefficient (R2) should NLT 0.999.