Development and validation of ultra-high-performance liquid chromatography-mass spectrometry method for the determination of raloxifene and its phase II metabolites in plasma : Application to pharmacokinetic studies in rats
© 2020 Wiley-VCH GmbH..
The aim of this study is to establish a reliable liquid chromatography-mass spectrometry method to simultaneously quantitate raloxifene, and its major metabolites, raloxifene-6-glucuronide, raloxifene-4'-glucuronide, and raloxifene-6-sulfate in rat plasma samples for pharmacokinetic studies. The separation of the analytes was achieved on a Waters BEH C18 column. Water (0.1% formic acid) and acetonitrile were used as the mobile phases for elution. A one-step protein precipitation using a mixture solvent was applied for plasma sample preparation. The method was validated following the FDA guidance. The results showed that the linear range were 1.95-1000 nM for raloxifene-6-glucuronide, and raloxifene-4'-glucuronide, 0.195-100 nM for raloxifene-6-sulfate, and 0.195-200 nM for raloxifene, respectively. The lower limit of quantification was 1.95, 1.95, 0.195, and 0.195 nM for raloxifene-6-glucuronide, raloxifene-4'-glucuronide, raloxifene-6-sulfate, and raloxifene, respectively. Only 20 µl of plasma sample was required since the method is sensitive. The intra- and interday variance is <15% and the accuracy is within 85-115%. The variance of matrix effect and recovery were <15%. The method was successfully applied in a pharmacokinetic study in rats with oral administration of raloxifene.
| Medienart: |
E-Artikel |
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| Erscheinungsjahr: |
2020 |
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| Erschienen: |
2020 |
| Enthalten in: |
Zur Gesamtaufnahme - volume:43 |
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| Enthalten in: |
Journal of separation science - 43(2020), 24 vom: 01. Dez., Seite 4414-4423 |
| Sprache: |
Englisch |
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| Beteiligte Personen: |
Du, Ting [VerfasserIn] |
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| Links: |
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| Themen: |
4F86W47BR6 |
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| Anmerkungen: |
Date Completed 20.09.2021 Date Revised 22.09.2021 published: Print-Electronic Citation Status MEDLINE |
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| doi: |
10.1002/jssc.202000835 |
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| funding: |
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| Förderinstitution / Projekttitel: |
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| PPN (Katalog-ID): |
NLM316877646 |
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| 245 | 1 | 0 | |a Development and validation of ultra-high-performance liquid chromatography-mass spectrometry method for the determination of raloxifene and its phase II metabolites in plasma |b Application to pharmacokinetic studies in rats |
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| 500 | |a published: Print-Electronic | ||
| 500 | |a Citation Status MEDLINE | ||
| 520 | |a © 2020 Wiley-VCH GmbH. | ||
| 520 | |a The aim of this study is to establish a reliable liquid chromatography-mass spectrometry method to simultaneously quantitate raloxifene, and its major metabolites, raloxifene-6-glucuronide, raloxifene-4'-glucuronide, and raloxifene-6-sulfate in rat plasma samples for pharmacokinetic studies. The separation of the analytes was achieved on a Waters BEH C18 column. Water (0.1% formic acid) and acetonitrile were used as the mobile phases for elution. A one-step protein precipitation using a mixture solvent was applied for plasma sample preparation. The method was validated following the FDA guidance. The results showed that the linear range were 1.95-1000 nM for raloxifene-6-glucuronide, and raloxifene-4'-glucuronide, 0.195-100 nM for raloxifene-6-sulfate, and 0.195-200 nM for raloxifene, respectively. The lower limit of quantification was 1.95, 1.95, 0.195, and 0.195 nM for raloxifene-6-glucuronide, raloxifene-4'-glucuronide, raloxifene-6-sulfate, and raloxifene, respectively. Only 20 µl of plasma sample was required since the method is sensitive. The intra- and interday variance is <15% and the accuracy is within 85-115%. The variance of matrix effect and recovery were <15%. The method was successfully applied in a pharmacokinetic study in rats with oral administration of raloxifene | ||
| 650 | 4 | |a Journal Article | |
| 650 | 4 | |a Validation Study | |
| 650 | 4 | |a chromatography | |
| 650 | 4 | |a mass spectrometry | |
| 650 | 4 | |a metabolites | |
| 650 | 4 | |a pharmacokinetic | |
| 650 | 4 | |a raloxifene | |
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| 700 | 1 | |a Sun, Rongjin |e verfasserin |4 aut | |
| 700 | 1 | |a Li, Li |e verfasserin |4 aut | |
| 700 | 1 | |a Ebuzoeme, Christabel |e verfasserin |4 aut | |
| 700 | 1 | |a Bui, Dinh |e verfasserin |4 aut | |
| 700 | 1 | |a Zheng, Zicong |e verfasserin |4 aut | |
| 700 | 1 | |a Yin, Taijun |e verfasserin |4 aut | |
| 700 | 1 | |a Liang, Dong |e verfasserin |4 aut | |
| 700 | 1 | |a Hu, Ming |e verfasserin |4 aut | |
| 700 | 1 | |a Gao, Song |e verfasserin |4 aut | |
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