Qualification

BP 606 T

1. Definition and general principles Qualification of UV-Visible spectrophotometer

2. Qualification When validation approach is related to a machine or equipment, rather than Validation, this is referred to as Qualification . Qualification is described as the action of proving that any premises, systems and items of equipment work correctly and actually lead to the expected results. It is the process used to establish confidence that the equipment is capable of consistently operating within established limits and tolerances

3. Qualification is often a part (initial state) of validation but the individual qualification steps alone do not constitute process validation Validation Process Instrument validation begins with a validation master plan that defines the steps in each process. Traditionally, these steps can be categorized into 4 separate qualification categories (DQ IQ OQ PQ ), which include:

4. Design Qualification (DQ) – The first step is to demonstrate whether the proposed design of the instrument can cope with the functional requirements of the end user. A proposed design must satisfy the DQ before construction and procurement of parts. Installation Qualification (IQ) – The instrument, with all its components and documentation, is placed correctly and checked for performance according to the requirements.

5. Operational Qualification (OQ) – All the major parts of the instrument are tested to ensure they all perform correctly and are in sync with the entire system. Performance Qualification (PQ) – The instrument is monitored over a period of time to check if it consistently delivers results within the required parameters.

6. Qualification of UV-Visible spectrophotometer

7. purpose The purpose of qualification is to provide test methodologies and acceptance criteria to ensure that the instrument is suitable for its intended use and that it will continue to function properly over extended time periods as part of PQ. A UV-Vis spectrophotometer must be qualified for both wavelength (x-axis) and photometric (y-axis, or signal axis) accuracy and precision, and the fundamental parameters of stray light and resolution must be established. OQ is carried out across the operational ranges required within the laboratory for both the absorbance and wavelength scales.

8. Installation Qualification The IQ requirements provide evidence that the hardware and software are properly installed in the desired location.

9. Operational & Performance qualification Following eight criteria should be verified with help of standard reference Wavelength Accuracy Stray Light Resolution Noise Baseline Flatness Stability Photometric Accuracy Linearity

10. Wavelength Accuracy Wavelength accuracy is defined as the deviation of the wavelength reading at an absorption band from the known wavelength of the band. • The wavelength deviation can cause significant errors in the qualitative and quantitative results of the UV–Vis measurement.

11. Protocol for Checking Wavelength Accuracy Wavelength accuracy verification is checked by measuring a known wave-length reference standard with well-characterized absorption or emission peaks and comparing the recorded wavelength of the peak(s) against the value (s) listed in the certificate of that reference standard. There are many standards that are commonly used to verify the wavelength accuracy of a spectrophotometer

12. Control of wavelengths Verify the wavelength scale using the absorption maxima of holmium perchlorate solution , the line of a hydrogen or deuterium discharge lamp or the lines of a mercury vapor arc shown below. 241.15 nm (Ho) 404.66 nm (Hg) 253.7 nm (Hg) 435.83 nm (Hg) 287.15 nm (Ho) 486.0 nm (Db) 302.25 nm (Hg) 486.1 nm ( Hb ) 313.16 nm (Hg) 536.3 nm (Ho) 334.15 nm (Hg) 546.07 nm (Hg) 361.5 nm (Ho) 576.96 nm (Hg) 365.48 nm (Hg) 579.07 nm (Hg)

13. Spectra of some commonly used wavelength standards such as a deuterium lamp, mercury vapour lamp, holmium oxide filter, and holmium oxide solution (4% holmium oxide in 10% perchloric acid in a 1-cm cell ). • Acceptance. ±1 nm in the UV range (200 to 380 nm) and ±3 nm in the visible range (380 to 800 nm). Three repeated scans of the same peak should be within ±0.5nm .

14. Stray Light Stray Light Stray light is defined as the detected light of any wavelength that is outside the bandwidth of the wavelength selected . • The causes for stray light are scattering, or poor instrument design. • Stray light causes a decrease in absorbance and reduces the linear range of the instrument. • High-absorbance measurements are affected more severely by stray light .

15. PROTOCOL For the stray light test, various cut-off filters or solutions can be used to estimate the stray light contribution, depending on the wavelengths is used. Scan the stray light testing solution in a 1-cm cell using air as the reference. The absorption of a solution of potassium chloride R (12 g/l) between 220 nm and 200 nm in a light path of 1 cm must rise suddenly and at a wavelength of 198 nm must be greater than 2 , measured against water R as a compensation liquid