Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in radiopharmaceutical
Objective: Analytical gas chromatography in line with a flame ionisation detector (GC-FID) method was developed and validated for evaluating organic solvents in radiopharmaceutical samples [18F]fluoro-ethyl-tyrosine ([18F]FET), [18F]fluoromisonidazole ([18F]FMISO) and [18F]fluorothymidine ([18F]FLT)...
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| Format: | Article |
| Language: | English |
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Elsevier
2021-09-01
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| Series: | Journal of King Saud University: Science |
| Subjects: | |
| Online Access: | http://www.sciencedirect.com/science/article/pii/S1018364721002159 |
| _version_ | 1819090564654563328 |
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| author | Hishar Hassan Muhamad Faiz Othman Zainul Amiruddin Zakaria Fathinul Fikri Ahmad Saad Hairil Rashmizal Abdul Razak |
| author_facet | Hishar Hassan Muhamad Faiz Othman Zainul Amiruddin Zakaria Fathinul Fikri Ahmad Saad Hairil Rashmizal Abdul Razak |
| author_sort | Hishar Hassan |
| collection | DOAJ |
| description | Objective: Analytical gas chromatography in line with a flame ionisation detector (GC-FID) method was developed and validated for evaluating organic solvents in radiopharmaceutical samples [18F]fluoro-ethyl-tyrosine ([18F]FET), [18F]fluoromisonidazole ([18F]FMISO) and [18F]fluorothymidine ([18F]FLT). Variables of the carrier gas flow (mL min−1) and a split ratio of injection on the response of analysis time and resolution were optimised with the assistance of a two-level full factorial design and desirability function of Derringer. Methods: The proposed procedure was validated following the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) Q2 (R1) guideline. Results: Excellent linearity, R2 > 0.990 indicated that approximately 99% of the variance in the response could be predicted from ethanol and acetonitrile concentrations ranging from 0.8 to 7.5 mg mL−1 and 0.1 to 1.0 mg mL−1, respectively. The proposed procedure proved to be selective, sensitive and accurate (85 to 105%), with excellent repeatability and precision (relative standard deviation (RSD) < 2%). In assessing the robustness of the method, the proposed procedure also proved to be robust as the standardised effects values (SE) were insignificant (p > 0.05). Conclusion: The proposed method has also been successfully used for the quantitative determination of ethanol and acetonitrile in [18F]FET, [18F]FMISO and [18F]FLT samples. Analytes were well resolved (R, 7.9 – 8.1) within 3.5 min even though the column had a larger, 0.53 mm internal diameter. The proposed method is, therefore, relevant for routine organic solvent quality control analysis of any 18F-radiopharmaceutical derivatives. |
| first_indexed | 2024-12-21T22:25:50Z |
| format | Article |
| id | doaj.art-884701e72d8b4b838206fde3c7c917e8 |
| institution | Directory Open Access Journal |
| issn | 1018-3647 |
| language | English |
| last_indexed | 2024-12-21T22:25:50Z |
| publishDate | 2021-09-01 |
| publisher | Elsevier |
| record_format | Article |
| series | Journal of King Saud University: Science |
| spelling | doaj.art-884701e72d8b4b838206fde3c7c917e82022-12-21T18:48:12ZengElsevierJournal of King Saud University: Science1018-36472021-09-01336101554Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in radiopharmaceuticalHishar Hassan0Muhamad Faiz Othman1Zainul Amiruddin Zakaria2Fathinul Fikri Ahmad Saad3Hairil Rashmizal Abdul Razak4Centre for Diagnostic Nuclear Imaging, Universiti Putra Malaysia, 43400 Serdang, Selangor, MalaysiaDepartment of Pharmacy Practice, Faculty of Pharmacy, Universiti Teknologi MARA, 42300 Bandar Puncak Alam, Selangor, MalaysiaDepartment of Biomedical Sciences, Faculty of Medicine & Health Sciences, Universiti Putra Malaysia, 43400 Serdang, Selangor, MalaysiaCentre for Diagnostic Nuclear Imaging, Universiti Putra Malaysia, 43400 Serdang, Selangor, Malaysia; Department of Radiology, Faculty of Medicine & Health Sciences, Universiti Putra Malaysia, 43400 Serdang, Selangor, MalaysiaCentre for Diagnostic Nuclear Imaging, Universiti Putra Malaysia, 43400 Serdang, Selangor, Malaysia; Department of Radiology, Faculty of Medicine & Health Sciences, Universiti Putra Malaysia, 43400 Serdang, Selangor, Malaysia; Corresponding author at: Department of Imaging, Faculty of Medicine & Health Sciences, Universiti Putra Malaysia, Serdang 43400, Malaysia.Objective: Analytical gas chromatography in line with a flame ionisation detector (GC-FID) method was developed and validated for evaluating organic solvents in radiopharmaceutical samples [18F]fluoro-ethyl-tyrosine ([18F]FET), [18F]fluoromisonidazole ([18F]FMISO) and [18F]fluorothymidine ([18F]FLT). Variables of the carrier gas flow (mL min−1) and a split ratio of injection on the response of analysis time and resolution were optimised with the assistance of a two-level full factorial design and desirability function of Derringer. Methods: The proposed procedure was validated following the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) Q2 (R1) guideline. Results: Excellent linearity, R2 > 0.990 indicated that approximately 99% of the variance in the response could be predicted from ethanol and acetonitrile concentrations ranging from 0.8 to 7.5 mg mL−1 and 0.1 to 1.0 mg mL−1, respectively. The proposed procedure proved to be selective, sensitive and accurate (85 to 105%), with excellent repeatability and precision (relative standard deviation (RSD) < 2%). In assessing the robustness of the method, the proposed procedure also proved to be robust as the standardised effects values (SE) were insignificant (p > 0.05). Conclusion: The proposed method has also been successfully used for the quantitative determination of ethanol and acetonitrile in [18F]FET, [18F]FMISO and [18F]FLT samples. Analytes were well resolved (R, 7.9 – 8.1) within 3.5 min even though the column had a larger, 0.53 mm internal diameter. The proposed method is, therefore, relevant for routine organic solvent quality control analysis of any 18F-radiopharmaceutical derivatives.http://www.sciencedirect.com/science/article/pii/S1018364721002159Organic solvent analysisQuality control analysisGas chromatography-FIDCarrier gas flowInjection split ratioRadiopharmaceutical |
| spellingShingle | Hishar Hassan Muhamad Faiz Othman Zainul Amiruddin Zakaria Fathinul Fikri Ahmad Saad Hairil Rashmizal Abdul Razak Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in radiopharmaceutical Journal of King Saud University: Science Organic solvent analysis Quality control analysis Gas chromatography-FID Carrier gas flow Injection split ratio Radiopharmaceutical |
| title | Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in radiopharmaceutical |
| title_full | Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in radiopharmaceutical |
| title_fullStr | Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in radiopharmaceutical |
| title_full_unstemmed | Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in radiopharmaceutical |
| title_short | Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in radiopharmaceutical |
| title_sort | multivariate optimisation and validation of the analytical gc fid for evaluating organic solvents in radiopharmaceutical |
| topic | Organic solvent analysis Quality control analysis Gas chromatography-FID Carrier gas flow Injection split ratio Radiopharmaceutical |
| url | http://www.sciencedirect.com/science/article/pii/S1018364721002159 |
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