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]fluoroethyl-tyrosine ([18F]FET [18F] fluoromisonidazole ([18F]FMISO) and [18F] fluorothymidine ([18F]FLT)....
| Main Authors: | , , , , |
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| Format: | Article |
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Elsevier
2021
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| Online Access: | http://psasir.upm.edu.my/id/eprint/94303/ |
| _version_ | 1848861960953659392 |
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| author | Hassan, Hishar Othman, Muhamad Faiz Zakaria, Zainul Amiruddin Ahmad Saad, Fathinul Fikri Abdul Razak, Hairil Rashmizal |
| author_facet | Hassan, Hishar Othman, Muhamad Faiz Zakaria, Zainul Amiruddin Ahmad Saad, Fathinul Fikri Abdul Razak, Hairil Rashmizal |
| author_sort | Hassan, Hishar |
| building | UPM Institutional Repository |
| collection | Online Access |
| 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]fluoroethyl-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 18Fradiopharmaceutical derivatives. |
| first_indexed | 2025-11-15T13:09:26Z |
| format | Article |
| id | upm-94303 |
| institution | Universiti Putra Malaysia |
| institution_category | Local University |
| last_indexed | 2025-11-15T13:09:26Z |
| publishDate | 2021 |
| publisher | Elsevier |
| recordtype | eprints |
| repository_type | Digital Repository |
| spelling | upm-943032023-05-08T03:06:07Z http://psasir.upm.edu.my/id/eprint/94303/ Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in radiopharmaceutical Hassan, Hishar Othman, Muhamad Faiz Zakaria, Zainul Amiruddin Ahmad Saad, Fathinul Fikri Abdul Razak, Hairil Rashmizal 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]fluoroethyl-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 18Fradiopharmaceutical derivatives. Elsevier 2021-09 Article PeerReviewed Hassan, Hishar and Othman, Muhamad Faiz and Zakaria, Zainul Amiruddin and Ahmad Saad, Fathinul Fikri and Abdul Razak, Hairil Rashmizal (2021) Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in radiopharmaceutical. Journal of King Saud University – Science, 33 (6). art. no. 101554. pp. 1-9. ISSN 1018-3647; ESSN: 2213-686X https://www.sciencedirect.com/science/article/pii/S1018364721002159?via%3Dihub 10.1016/j.jksus.2021.101554 |
| spellingShingle | Hassan, Hishar Othman, Muhamad Faiz Zakaria, Zainul Amiruddin Ahmad Saad, Fathinul Fikri Abdul Razak, Hairil Rashmizal Multivariate optimisation and validation of the analytical GC-FID for evaluating organic solvents in 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 |
| url | http://psasir.upm.edu.my/id/eprint/94303/ http://psasir.upm.edu.my/id/eprint/94303/ http://psasir.upm.edu.my/id/eprint/94303/ |