The analysis of major impurities of lipophilic-conjugated phosphorothioate oligonucleotides by ion-pair reversed-phase HPLC combined with MALDI-TOF-MS
Identifieur interne : 001146 ( Istex/Curation ); précédent : 001145; suivant : 001147The analysis of major impurities of lipophilic-conjugated phosphorothioate oligonucleotides by ion-pair reversed-phase HPLC combined with MALDI-TOF-MS
Auteurs : Cai-Hong Liu [République populaire de Chine] ; Dan-Dan Lu [République populaire de Chine] ; Xin-Xiu Deng [République populaire de Chine] ; Ying Wang [République populaire de Chine] ; Jing-Yu Zhang [République populaire de Chine] ; Yu-Lin Zhang [République populaire de Chine] ; Sheng-Qi Wang [République populaire de Chine]Source :
- Analytical and Bioanalytical Chemistry [ 1618-2642 ] ; 2012-05-01.
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Abstract
Abstract: A simple and rapid ion-pair reversed phase high-performance liquid chromatography (IP-RP-HPLC) method was developed to analyse the major impurities of lipophilic-conjugated phosphorothioate oligonucleotides (ODNs), which provided better separation performance than capillary gel electrophoresis and ion exchange chromatograph methods. The study showed that covalent conjugations of lipophilic group (docosanyl, C22) to ODN at 5′-termini (denoted as 5′C22-Flu) or 3′-termini (denoted as 3′C22-Flu) exhibited similar chromatographic retention behavior. Some important analytical conditions of IP-RP-HPLC, including column type, ion-pairing buffer composition, and separation temperature, were investigated for the effects on the separation of crude 5′C22-Flu. As expected, the method developed was successfully applied to the analysis of crude 3′C22-Flu and both purified products. Furthermore, the related impurities derived from the synthetic process were identified by matrix-assisted laser desorption-ionization time-of-flight mass spectrum. These MS results are of benefit to understanding the major process-related impurities in lipophilic-ODN conjugates synthesis, thereby elevating the quality of target products.
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DOI: 10.1007/s00216-012-5935-5
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combined with MALDI-TOF-MS</title><author><name sortKey="Liu, Cai Hong" sort="Liu, Cai Hong" uniqKey="Liu C" first="Cai-Hong" last="Liu">Cai-Hong Liu</name><affiliation wicri:level="1"><mods:affiliation>Chinese PLA Postgraduate Medical School, 100853, Beijing, China</mods:affiliation><country xml:lang="fr">République populaire de Chine</country><wicri:regionArea>Chinese PLA Postgraduate Medical School, 100853, Beijing</wicri:regionArea></affiliation><affiliation wicri:level="1"><mods:affiliation>Beijing Institute of Radiation Medicine, 100850, Beijing, China</mods:affiliation><country xml:lang="fr">République populaire de Chine</country><wicri:regionArea>Beijing Institute of Radiation Medicine, 100850, Beijing</wicri:regionArea></affiliation></author><author><name sortKey="Lu, Dan Dan" sort="Lu, Dan Dan" uniqKey="Lu D" first="Dan-Dan" last="Lu">Dan-Dan Lu</name><affiliation wicri:level="1"><mods:affiliation>Beijing Institute of Radiation Medicine, 100850, Beijing, 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Chine</country></affiliation></author></analytic><monogr></monogr><series><title level="j">Analytical and Bioanalytical Chemistry</title><title level="j" type="abbrev">Anal Bioanal Chem</title><idno type="ISSN">1618-2642</idno><idno type="eISSN">1618-2650</idno><imprint><publisher>Springer-Verlag</publisher><pubPlace>Berlin/Heidelberg</pubPlace><date type="published" when="2012-05-01">2012-05-01</date><biblScope unit="volume">403</biblScope><biblScope unit="issue">5</biblScope><biblScope unit="page" from="1333">1333</biblScope><biblScope unit="page" to="1342">1342</biblScope></imprint><idno type="ISSN">1618-2642</idno></series></biblStruct></sourceDesc><seriesStmt><idno type="ISSN">1618-2642</idno></seriesStmt></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Analysis of major impurities</term><term>Ion-pair reversed-phase HPLC</term><term>Lipophilic-conjugated phosphorothioate oligonucleotides</term><term>MALDL-TOF-MS</term></keywords></textClass><langUsage><language ident="en">en</language></langUsage></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">Abstract: A simple and rapid ion-pair reversed phase high-performance liquid chromatography (IP-RP-HPLC) method was developed to analyse the major impurities of lipophilic-conjugated phosphorothioate oligonucleotides (ODNs), which provided better separation performance than capillary gel electrophoresis and ion exchange chromatograph methods. The study showed that covalent conjugations of lipophilic group (docosanyl, C22) to ODN at 5′-termini (denoted as 5′C22-Flu) or 3′-termini (denoted as 3′C22-Flu) exhibited similar chromatographic retention behavior. Some important analytical conditions of IP-RP-HPLC, including column type, ion-pairing buffer composition, and separation temperature, were investigated for the effects on the separation of crude 5′C22-Flu. As expected, the method developed was successfully applied to the analysis of crude 3′C22-Flu and both purified products. Furthermore, the related impurities derived from the synthetic process were identified by matrix-assisted laser desorption-ionization time-of-flight mass spectrum. These MS results are of benefit to understanding the major process-related impurities in lipophilic-ODN conjugates synthesis, thereby elevating the quality of target products.</div></front></TEI></record>Pour manipuler ce document sous Unix (Dilib)
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