System suitability requirements, setting

System suitability requirements for retention time, efficiency, resolution, and tailing factor are set based on prior method challenging experiments and prior method development experience. This is a dynamic process and as the user gains more experience with the method, the breadth of the acceptance criteria is further expanded until the method is finally validated for the intended purpose. 

Good Laboratory Practice (GLP) The system provides a comprehensive feature set to aid customers in meeting GLP requirements. This includes features such as certificate-of-software validation, user-access levels, instrument and sequence logbooks, system-suitability software for aU supported HP instruments, standard GLP reports, and a GLP save option that encrypts and saves data and methods together. 

Considering the importance of system suitability in determining the accuracy and reliability of method results, it is improper to set an RSD requirement of < 2% for a method that consistently yields values of < 1%. If peak tailing is always < 1.5, then a requirement of < 2.0 does not provide feedback to notify the chemist of a poor or failing column. Resolution requirements must be required for the critical pair of components where a loss of resolution would impact method performance. By addressing these parameters with a more critical eye, the suitability of the analysis system can be accurately determined. 

H-bonded systems may require additional diffuse or polarization functions. For example, the 6-311++G(d,p) basis set had been found to be suitable for H-bonded systems [78-81], It may be necessary to include Basis Set Superposition Errors (BSSE) [82] and Zero-Point-Energy (ZPE) corrections in evaluating the relative stabilities. Such corrections are often of the same magnitude as the energy differences among the dominant conformers. Moreover, the relative conformer energies may also differ noticeably with the basis sets used. All these factors will affect the Boltzmann factors predicted for different conformers and therefore the appearance of the population weighted VA and VCD spectra. Thus, an appropriate selection of DFT functionals and basis sets is very important for VCD simulations. A scale factor of 0.97-0.98 is usually applied to the calculated harmonic frequencies to account for the fact that the observed frequencies arise from an anharmonic force field instead of a harmonic one. A Lorentzian line shape is typically used in simulations of VA and VCD spectra. The full-width at half maximum (FWHM) used in the spectral simulation is usually based on the experimental VA line widths. 

The extended Hiickel approach has proved to be rather successful for such a simple theory for example, the famous Woodward-Hoffmann rules (see Section 5.9.4) were based upon calculations using this model. Extended Hiickel theory has found particular application in those areas where alternative theories cannot be used. This is largely due to the fact that the basis set requires no more than experimentally determined ionisation potentials. It is particularly useful for studying systems containing metals these systems are problematic for many other methods due to the lack of suitable basis sets. 

A number of aqueous liquid crystalline media suitable for inducing a weak ahgn-ment of biomolecules are known [405]. It should be understood that the choice for a particular liquid crystalline system depends on the properties of the biomolecule, liquid crystalline particles and temperature, ionic strength and eventual co-sol-vents. Some of the critical factors affecting the formation of the Hquid crystal and the size and direction of the solute alignment may be difficult to anticipate beforehand and preliminary experiments are often required to find a suitable system. Furthermore, the set of aqueous liquid crystals for aligning biomolecules is likely to continue to expand as the search for novel media is currently in progress. 

Although all aspects of the computer system should be maintained under an appropriate level of eonfiguration control, it should be considered whether some part of the system (for example set points) should be more easily changeable than other parts. If so, requirements for a suitable means of achieving this should be specified... 

Validation requires analytical method instructions comprising a system suitability test in order to verify identical starting conditions. Part or full revalidation may be considered if system suitability tests, or the results of quality control sample analysis, are out of pre-set acceptance criteria and the source of the error cannot be tracked back to instrumental factors or anything else. 

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