Comparison of the NMR and the Acid Value Determination Methods for Quality Control of Input Polysorbates
Polysorbates (PS) are the most common non-ionic surfactants used in protein formulations. Their degradation has been studied intensively in recent years. Ester bond hydrolysis is one of many pathways of PS degradation that can lead to accumulation of free fatty acids (FFAs) and particle formation. T...
| Main Authors: | , , , |
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| Format: | Article |
| Language: | English |
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Slovenian Chemical Society
2019-12-01
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| Series: | Acta Chimica Slovenica |
| Subjects: | |
| Online Access: | https://journals.matheo.si/index.php/ACSi/article/view/5144 |
| _version_ | 1818580756434255872 |
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| author | Ema Valentina Brovč Stane Pajk Roman Šink Janez Mravljak |
| author_facet | Ema Valentina Brovč Stane Pajk Roman Šink Janez Mravljak |
| author_sort | Ema Valentina Brovč |
| collection | DOAJ |
| description | Polysorbates (PS) are the most common non-ionic surfactants used in protein formulations. Their degradation has been studied intensively in recent years. Ester bond hydrolysis is one of many pathways of PS degradation that can lead to accumulation of free fatty acids (FFAs) and particle formation. The distribution and quantity of FFAs in PSs impacts directly on product quality. Characterization of input PS is highly relevant, because the initial content of FFAs differs greatly between manufacturers. The purpose of this study was to set up a quick and simple analytical method for the quantitative evaluation of FFAs in PS. The content of FFAs was measured for selected PS 20 and 80, using two methods, 1H nuclear magnetic resonance spectroscopy (1H NMR) and the European pharmacopoeia method for determining acid value (IA). These methods have been evaluated using the method of standard addition and, based on the results, they are interchangeable. It was concluded that 1H NMR is a useful tool for quality control of input PS and a rapid method for indicating the rate of PS degradation by hydrolysis and oxidation. Further, a newly discovered impurity in PS raw material, the long chain ketone 12-tricosanone, can be identified using 1H NMR. |
| first_indexed | 2024-12-16T07:22:39Z |
| format | Article |
| id | doaj.art-8a490486103746379735e7bbf518ad74 |
| institution | Directory Open Access Journal |
| issn | 1318-0207 1580-3155 |
| language | English |
| last_indexed | 2024-12-16T07:22:39Z |
| publishDate | 2019-12-01 |
| publisher | Slovenian Chemical Society |
| record_format | Article |
| series | Acta Chimica Slovenica |
| spelling | doaj.art-8a490486103746379735e7bbf518ad742022-12-21T22:39:35ZengSlovenian Chemical SocietyActa Chimica Slovenica1318-02071580-31552019-12-0166493494310.17344/acsi.2019.5144763Comparison of the NMR and the Acid Value Determination Methods for Quality Control of Input PolysorbatesEma Valentina Brovč0Stane Pajk1Roman Šink2Janez Mravljak3University of Ljubljana, Faculty of Pharmacy, Aškerčeva 7, SI-1000 Ljubljana, Slovenia Lek d.d., Kolodvorska 27, SI-1234 Mengeš, SloveniaUniversity of Ljubljana, Faculty of Pharmacy, Aškerčeva 7, SI-1000 Ljubljana, SloveniaLek d.d., Kolodvorska 27, SI-1234 Mengeš, SloveniaUniversity of Ljubljana, Faculty of Pharmacy, Aškerčeva 7, SI-1000 Ljubljana, SloveniaPolysorbates (PS) are the most common non-ionic surfactants used in protein formulations. Their degradation has been studied intensively in recent years. Ester bond hydrolysis is one of many pathways of PS degradation that can lead to accumulation of free fatty acids (FFAs) and particle formation. The distribution and quantity of FFAs in PSs impacts directly on product quality. Characterization of input PS is highly relevant, because the initial content of FFAs differs greatly between manufacturers. The purpose of this study was to set up a quick and simple analytical method for the quantitative evaluation of FFAs in PS. The content of FFAs was measured for selected PS 20 and 80, using two methods, 1H nuclear magnetic resonance spectroscopy (1H NMR) and the European pharmacopoeia method for determining acid value (IA). These methods have been evaluated using the method of standard addition and, based on the results, they are interchangeable. It was concluded that 1H NMR is a useful tool for quality control of input PS and a rapid method for indicating the rate of PS degradation by hydrolysis and oxidation. Further, a newly discovered impurity in PS raw material, the long chain ketone 12-tricosanone, can be identified using 1H NMR.https://journals.matheo.si/index.php/ACSi/article/view/5144nuclear magnetic resonanceacid numberfatty acidspolysorbatesdegradation |
| spellingShingle | Ema Valentina Brovč Stane Pajk Roman Šink Janez Mravljak Comparison of the NMR and the Acid Value Determination Methods for Quality Control of Input Polysorbates Acta Chimica Slovenica nuclear magnetic resonance acid number fatty acids polysorbates degradation |
| title | Comparison of the NMR and the Acid Value Determination Methods for Quality Control of Input Polysorbates |
| title_full | Comparison of the NMR and the Acid Value Determination Methods for Quality Control of Input Polysorbates |
| title_fullStr | Comparison of the NMR and the Acid Value Determination Methods for Quality Control of Input Polysorbates |
| title_full_unstemmed | Comparison of the NMR and the Acid Value Determination Methods for Quality Control of Input Polysorbates |
| title_short | Comparison of the NMR and the Acid Value Determination Methods for Quality Control of Input Polysorbates |
| title_sort | comparison of the nmr and the acid value determination methods for quality control of input polysorbates |
| topic | nuclear magnetic resonance acid number fatty acids polysorbates degradation |
| url | https://journals.matheo.si/index.php/ACSi/article/view/5144 |
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