Validation of the ICP-MS Method for Determination of Trace Elements Provided by ICH Q3D Guideline in Fosamprenavir Calcium
Fosamprenavir calcium is an active pharmaceutical ingredient (API) in which trace elements must be monitored by ICH Q3D Guideline. It delivers appropriate method to ensure the quality of the product and its safe use. Elemental impurities in API are separated in three classes based on their toxicity...
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Croatian Society of Chemical Engineers
2021
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oai:doaj.org-article:45a2082285ce45c18835972eff2dd6db2021-11-03T23:33:59ZValidation of the ICP-MS Method for Determination of Trace Elements Provided by ICH Q3D Guideline in Fosamprenavir Calcium10.15255/KUI.2021.0040022-98301334-9090https://doaj.org/article/45a2082285ce45c18835972eff2dd6db2021-11-01T00:00:00Zhttp://silverstripe.fkit.hr/kui/assets/Uploads/7-701-709-KUI-11-12-2021.pdfhttps://doaj.org/toc/0022-9830https://doaj.org/toc/1334-9090Fosamprenavir calcium is an active pharmaceutical ingredient (API) in which trace elements must be monitored by ICH Q3D Guideline. It delivers appropriate method to ensure the quality of the product and its safe use. Elemental impurities in API are separated in three classes based on their toxicity and probability of their occurrence in the product. ICP-MS has proven to be a suitable technique with the appropriate sample preparation method. Due to the presence of oxidising agents in the sample preparation, determination of osmium is problematic. In the presence of oxidising nitric acid, a highly volatile and toxic osmium tetraoxide is formed. Due to its high volatility, the recovery of osmium has reached the value of 287 %, which exceeds recovery limit (70–150 %). However, osmium can be stabilised by complexation with thiourea in the hydrochloric acid solution (recovery = 87 %). In that way, the loss of osmium is reduced and good results are achieved in terms of usability, accuracy, and precision. A method with addition of thiourea has been successfully validated through main validation parameters: linearity, quantitation limit, selectivity, accuracy, precision (which included repeatability and intralaboratory reproducibility), and robustness. Each of these validation parameters met the acceptance criteria, and therefore it was concluded that the method is suitable for the determination of trace elements in fosamprenavir calcium by ICP-MS.Irena RadićMislav RunjeMatija CvetnićMaja HalužanMario-Livio JeličićMartina MiloložaDajana Kučić GrgićViktorija PrevarićŠime UkićTomislav BolančaCroatian Society of Chemical Engineersarticlemicrowave digestionicp-msapifosamprenavir calciumosmiumChemistryQD1-999ENHRKemija u Industriji, Vol 70, Iss 11-12, Pp 701-709 (2021) |
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microwave digestion icp-ms api fosamprenavir calcium osmium Chemistry QD1-999 |
| spellingShingle |
microwave digestion icp-ms api fosamprenavir calcium osmium Chemistry QD1-999 Irena Radić Mislav Runje Matija Cvetnić Maja Halužan Mario-Livio Jeličić Martina Miloloža Dajana Kučić Grgić Viktorija Prevarić Šime Ukić Tomislav Bolanča Validation of the ICP-MS Method for Determination of Trace Elements Provided by ICH Q3D Guideline in Fosamprenavir Calcium |
| description |
Fosamprenavir calcium is an active pharmaceutical ingredient (API) in which trace elements must be monitored by ICH Q3D Guideline. It delivers appropriate method to ensure the quality of the product and its safe use. Elemental impurities in API are separated in three classes based on their toxicity and probability of their occurrence in the product. ICP-MS has proven to be a suitable technique with the appropriate sample preparation method. Due to the presence of oxidising agents in the sample preparation, determination of osmium is problematic. In the presence of oxidising nitric acid, a highly volatile and toxic osmium tetraoxide is formed. Due to its high volatility, the recovery of osmium has reached the value of 287 %, which exceeds recovery limit (70–150 %). However, osmium can be stabilised by complexation with thiourea in the hydrochloric acid solution (recovery = 87 %). In that way, the loss of osmium is reduced and good results are achieved in terms of usability, accuracy, and precision.
A method with addition of thiourea has been successfully validated through main validation parameters: linearity, quantitation limit, selectivity, accuracy, precision (which included repeatability and intralaboratory reproducibility), and robustness. Each of these validation parameters met the acceptance criteria, and therefore it was concluded that the method is suitable for the determination of trace elements in fosamprenavir calcium by ICP-MS. |
| format |
article |
| author |
Irena Radić Mislav Runje Matija Cvetnić Maja Halužan Mario-Livio Jeličić Martina Miloloža Dajana Kučić Grgić Viktorija Prevarić Šime Ukić Tomislav Bolanča |
| author_facet |
Irena Radić Mislav Runje Matija Cvetnić Maja Halužan Mario-Livio Jeličić Martina Miloloža Dajana Kučić Grgić Viktorija Prevarić Šime Ukić Tomislav Bolanča |
| author_sort |
Irena Radić |
| title |
Validation of the ICP-MS Method for Determination of Trace Elements Provided by ICH Q3D Guideline in Fosamprenavir Calcium |
| title_short |
Validation of the ICP-MS Method for Determination of Trace Elements Provided by ICH Q3D Guideline in Fosamprenavir Calcium |
| title_full |
Validation of the ICP-MS Method for Determination of Trace Elements Provided by ICH Q3D Guideline in Fosamprenavir Calcium |
| title_fullStr |
Validation of the ICP-MS Method for Determination of Trace Elements Provided by ICH Q3D Guideline in Fosamprenavir Calcium |
| title_full_unstemmed |
Validation of the ICP-MS Method for Determination of Trace Elements Provided by ICH Q3D Guideline in Fosamprenavir Calcium |
| title_sort |
validation of the icp-ms method for determination of trace elements provided by ich q3d guideline in fosamprenavir calcium |
| publisher |
Croatian Society of Chemical Engineers |
| publishDate |
2021 |
| url |
https://doaj.org/article/45a2082285ce45c18835972eff2dd6db |
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