ISO_NWIPs-for-Ballot

ISO/NP

832

9 Quality assurance requirements 9.1 General 833 To manage the quality of the data, records shall be kept of the reference material for qNMR, the NMR 834 spectrum baseline and signal line shape, and the apparatus performance records shall be kept of the 835 source, certificate of analysis and certification report and source of SI-traceability of the reference 836 material for qNMR". 837 For the assessment results, the raw data (FID data, spectral data), the measurement records and NMR 838 spectra shall be archived along with the test report and electronic files. 839 The content of such records should cover all details that are considered appropriate to be included in 840 the standard operating procedures (SOP) for each individual analysis method. Thus the appropriate 841 items should be selected and defined. 842 9.2 Qualification of the NMR apparatus 843 To confirm the suitability of the NMR apparatus, two areas shall be assessed: the suitability of the 844 apparatus itself, and the suitability of the apparatus with regard to the qNMR measurements. 845 a) Periodic and routine inspections 846 Periodic or routine inspections shall be performed to ensure that the established specifications 847 (performance) of the apparatus are satisfied, as described in 6.6. 848 b) Suitability of the qNMR measurements 849 Performance management of the NMR apparatus shall be implemented to confirm that the NMR 850 apparatus used is suitable with regard to the 1 H qNMR measurements. In this case, confirm that 851 the signal area for the measurement target can be accurately quantified within the spectrum 852 width where the signal is observed. When performing measurements under 1 H qNMR 853 measurement conditions using an extremely high purity (≥99,5 %) compound which does not 854 contain significant amounts of impurities with similar structures, always verify that the ratio of 855 the multiple signals acquired from the compound accurately matches the theoretical ratio of the 856 signal areas. 857 It is recommended to use test target species that have certified purity values. 858 9.3 System suitability test 859 9.3.1 General 860 For the measurement of the purity or content of an analyte, confirm that 9.3.2 to 9.3.4 below are applied 861 to obtain the desired quantitative accuracy. However, if requirements for the system suitability are 862 specified in any standards, those shall apply. Otherwise, tests shall be performed and the results shall 863 be evaluated. 864 865 9.3.2 System repeatability for system suitability test 866 When measurements are repeated with a sample solution under 1 H qNMR measurement conditions, 867 confirm that the ratios between the area of each signal used for quantification of the analyte and the 868 area of the signal for the qNMR standard reference material are constant. 869

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