Stability Indicating LC Method Development for Hydroxychloroquine Sulfate Impurities as Available for Treatment of COVID-19 and Evaluation of Risk Assessment Prior to Method Validation by Quality by Design Approach.
Identifieur interne : 000D46 ( Main/Corpus ); précédent : 000D45; suivant : 000D47Stability Indicating LC Method Development for Hydroxychloroquine Sulfate Impurities as Available for Treatment of COVID-19 and Evaluation of Risk Assessment Prior to Method Validation by Quality by Design Approach.
Auteurs : Thirupathi Dongala ; Naresh Kumar Katari ; Ashok Kumar Palakurthi ; Lakshmi Narasimha Rao Katakam ; Vishnu Murthy MarisettiSource :
- Chromatographia [ 0009-5893 ] ; 2020.
Abstract
A quality by design-based stability indicating HPLC method has been developed for hydroxychloroquine sulfate impurities. The optimized HPLC method can detect and quantify the hydroxychloroquine sulfate and related organic impurities in pharmaceutical solid oral dosage forms. Nowadays, for the quantification of impurities in drug products demands more comprehensive way of analytical method development. The quality by design approach allows the assessment of different analytical parameters and their effects with minimum number of experiments. A highly sensitive and stability indicating RP-HPLC method was developed and evaluated the risk assessment prior to method validation. The chromatographic separation was achieved with X-terra phenyl column (250 × 4.6 mm, 5 µm) using phosphate buffer (0.3 M and pH 2.5). The gradient method flow rate was 1.5 mL min-1 and UV detection was made at 220 nm. The calibration curve of hydroxychloroquine sulfate and related impurities were linear from LOQ to 150% and correlation coefficient was found more than 0.999. The precision and intermediate precision % RSD values were found less than 2.0. In all forced degradation conditions, the purity angle of HCQ was found less than purity threshold. The optimized method found to be specific, accurate, rugged, and robust for determination of hydroxychloroquine sulfate impurities in the solid oral dosage forms. Finally, the method was applied successfully in quality control lab for stability analysis.
DOI: 10.1007/s10337-020-03945-5
PubMed: 32863397
PubMed Central: PMC7445446
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Stability Indicating LC Method Development for Hydroxychloroquine Sulfate Impurities as Available for Treatment of COVID-19 and Evaluation of Risk Assessment Prior to Method Validation by Quality by Design Approach.</title><author><name sortKey="Dongala, Thirupathi" sort="Dongala, Thirupathi" uniqKey="Dongala T" first="Thirupathi" last="Dongala">Thirupathi Dongala</name><affiliation><nlm:affiliation>Analytical Research and Development, Aurex Laboratories LLC, 10 lake drive, East windsor, New Jersey 08520 USA.</nlm:affiliation></affiliation><affiliation><nlm:affiliation>Department of Chemistry, GITAM University, Hyderabad, Telangana 502329 India.</nlm:affiliation></affiliation></author><author><name sortKey="Katari, Naresh Kumar" sort="Katari, Naresh Kumar" uniqKey="Katari N" first="Naresh Kumar" last="Katari">Naresh Kumar Katari</name><affiliation><nlm:affiliation>Department of Chemistry, GITAM University, Hyderabad, Telangana 502329 India.</nlm:affiliation></affiliation></author><author><name sortKey="Palakurthi, Ashok Kumar" sort="Palakurthi, Ashok Kumar" uniqKey="Palakurthi A" first="Ashok Kumar" last="Palakurthi">Ashok Kumar Palakurthi</name><affiliation><nlm:affiliation>Analytical Research and Development, Aurex Laboratories LLC, 10 lake drive, East windsor, New Jersey 08520 USA.</nlm:affiliation></affiliation></author><author><name sortKey="Katakam, Lakshmi Narasimha Rao" sort="Katakam, Lakshmi Narasimha Rao" uniqKey="Katakam L" first="Lakshmi Narasimha Rao" last="Katakam">Lakshmi Narasimha Rao Katakam</name><affiliation><nlm:affiliation>Analytical Development, Saptalis Pharmaceuticals LLC, Hauppauge, NY 11788 USA.</nlm:affiliation></affiliation></author><author><name sortKey="Marisetti, Vishnu Murthy" sort="Marisetti, Vishnu Murthy" uniqKey="Marisetti V" first="Vishnu Murthy" last="Marisetti">Vishnu Murthy Marisetti</name><affiliation><nlm:affiliation>Analytical Research and Development, ScieGen Pharmaceuticals Inc, 89 Arkay drive, Hauppauge, NY 11788 USA.</nlm:affiliation></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">PubMed</idno><date when="2020">2020</date><idno type="RBID">pubmed:32863397</idno><idno type="pmid">32863397</idno><idno type="doi">10.1007/s10337-020-03945-5</idno><idno type="pmc">PMC7445446</idno><idno type="wicri:Area/Main/Corpus">000D46</idno><idno type="wicri:explorRef" wicri:stream="Main" wicri:step="Corpus" wicri:corpus="PubMed">000D46</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en">Stability Indicating LC Method Development for Hydroxychloroquine Sulfate Impurities as Available for Treatment of COVID-19 and Evaluation of Risk Assessment Prior to Method Validation by Quality by Design Approach.</title><author><name sortKey="Dongala, Thirupathi" sort="Dongala, Thirupathi" uniqKey="Dongala T" first="Thirupathi" last="Dongala">Thirupathi Dongala</name><affiliation><nlm:affiliation>Analytical Research and Development, Aurex Laboratories LLC, 10 lake drive, East windsor, New Jersey 08520 USA.</nlm:affiliation></affiliation><affiliation><nlm:affiliation>Department of Chemistry, GITAM University, Hyderabad, Telangana 502329 India.</nlm:affiliation></affiliation></author><author><name sortKey="Katari, Naresh Kumar" sort="Katari, Naresh Kumar" uniqKey="Katari N" first="Naresh Kumar" last="Katari">Naresh Kumar Katari</name><affiliation><nlm:affiliation>Department of Chemistry, GITAM University, Hyderabad, Telangana 502329 India.</nlm:affiliation></affiliation></author><author><name sortKey="Palakurthi, Ashok Kumar" sort="Palakurthi, Ashok Kumar" uniqKey="Palakurthi A" first="Ashok Kumar" last="Palakurthi">Ashok Kumar Palakurthi</name><affiliation><nlm:affiliation>Analytical Research and Development, Aurex Laboratories LLC, 10 lake drive, East windsor, New Jersey 08520 USA.</nlm:affiliation></affiliation></author><author><name sortKey="Katakam, Lakshmi Narasimha Rao" sort="Katakam, Lakshmi Narasimha Rao" uniqKey="Katakam L" first="Lakshmi Narasimha Rao" last="Katakam">Lakshmi Narasimha Rao Katakam</name><affiliation><nlm:affiliation>Analytical Development, Saptalis Pharmaceuticals LLC, Hauppauge, NY 11788 USA.</nlm:affiliation></affiliation></author><author><name sortKey="Marisetti, Vishnu Murthy" sort="Marisetti, Vishnu Murthy" uniqKey="Marisetti V" first="Vishnu Murthy" last="Marisetti">Vishnu Murthy Marisetti</name><affiliation><nlm:affiliation>Analytical Research and Development, ScieGen Pharmaceuticals Inc, 89 Arkay drive, Hauppauge, NY 11788 USA.</nlm:affiliation></affiliation></author></analytic><series><title level="j">Chromatographia</title><idno type="ISSN">0009-5893</idno><imprint><date when="2020" type="published">2020</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">A quality by design-based stability indicating HPLC method has been developed for hydroxychloroquine sulfate impurities. The optimized HPLC method can detect and quantify the hydroxychloroquine sulfate and related organic impurities in pharmaceutical solid oral dosage forms. Nowadays, for the quantification of impurities in drug products demands more comprehensive way of analytical method development. The quality by design approach allows the assessment of different analytical parameters and their effects with minimum number of experiments. A highly sensitive and stability indicating RP-HPLC method was developed and evaluated the risk assessment prior to method validation. The chromatographic separation was achieved with X-terra phenyl column (250 × 4.6 mm, 5 µm) using phosphate buffer (0.3 M and pH 2.5). The gradient method flow rate was 1.5 mL min<sup>-1</sup> and UV detection was made at 220 nm. The calibration curve of hydroxychloroquine sulfate and related impurities were linear from LOQ to 150% and correlation coefficient was found more than 0.999. The precision and intermediate precision % RSD values were found less than 2.0. In all forced degradation conditions, the purity angle of HCQ was found less than purity threshold. The optimized method found to be specific, accurate, rugged, and robust for determination of hydroxychloroquine sulfate impurities in the solid oral dosage forms. Finally, the method was applied successfully in quality control lab for stability analysis.</div></front></TEI><pubmed><MedlineCitation Status="Publisher" Owner="NLM"><PMID Version="1">32863397</PMID><DateRevised><Year>2020</Year><Month>09</Month><Day>28</Day></DateRevised><Article PubModel="Print-Electronic"><Journal><ISSN IssnType="Print">0009-5893</ISSN><JournalIssue CitedMedium="Print"><PubDate><Year>2020</Year><Month>Aug</Month><Day>25</Day></PubDate></JournalIssue><Title>Chromatographia</Title><ISOAbbreviation>Chromatographia</ISOAbbreviation></Journal><ArticleTitle>Stability Indicating LC Method Development for Hydroxychloroquine Sulfate Impurities as Available for Treatment of COVID-19 and Evaluation of Risk Assessment Prior to Method Validation by Quality by Design Approach.</ArticleTitle><Pagination><MedlinePgn>1-13</MedlinePgn></Pagination><ELocationID EIdType="doi" ValidYN="Y">10.1007/s10337-020-03945-5</ELocationID><Abstract><AbstractText>A quality by design-based stability indicating HPLC method has been developed for hydroxychloroquine sulfate impurities. The optimized HPLC method can detect and quantify the hydroxychloroquine sulfate and related organic impurities in pharmaceutical solid oral dosage forms. Nowadays, for the quantification of impurities in drug products demands more comprehensive way of analytical method development. The quality by design approach allows the assessment of different analytical parameters and their effects with minimum number of experiments. A highly sensitive and stability indicating RP-HPLC method was developed and evaluated the risk assessment prior to method validation. The chromatographic separation was achieved with X-terra phenyl column (250 × 4.6 mm, 5 µm) using phosphate buffer (0.3 M and pH 2.5). The gradient method flow rate was 1.5 mL min<sup>-1</sup> and UV detection was made at 220 nm. The calibration curve of hydroxychloroquine sulfate and related impurities were linear from LOQ to 150% and correlation coefficient was found more than 0.999. The precision and intermediate precision % RSD values were found less than 2.0. In all forced degradation conditions, the purity angle of HCQ was found less than purity threshold. The optimized method found to be specific, accurate, rugged, and robust for determination of hydroxychloroquine sulfate impurities in the solid oral dosage forms. Finally, the method was applied successfully in quality control lab for stability analysis.</AbstractText><CopyrightInformation>© Springer-Verlag GmbH Germany, part of Springer Nature 2020.</CopyrightInformation></Abstract><AuthorList CompleteYN="Y"><Author ValidYN="Y"><LastName>Dongala</LastName><ForeName>Thirupathi</ForeName><Initials>T</Initials><Identifier Source="ORCID">0000-0001-8251-5005</Identifier><AffiliationInfo><Affiliation>Analytical Research and Development, Aurex Laboratories LLC, 10 lake drive, East windsor, New Jersey 08520 USA.</Affiliation></AffiliationInfo><AffiliationInfo><Affiliation>Department of Chemistry, GITAM University, Hyderabad, Telangana 502329 India.</Affiliation><Identifier Source="GRID">grid.411710.2</Identifier><Identifier Source="ISNI">0000 0004 0497 3037</Identifier></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Katari</LastName><ForeName>Naresh Kumar</ForeName><Initials>NK</Initials><AffiliationInfo><Affiliation>Department of Chemistry, GITAM University, Hyderabad, Telangana 502329 India.</Affiliation><Identifier Source="GRID">grid.411710.2</Identifier><Identifier Source="ISNI">0000 0004 0497 3037</Identifier></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Palakurthi</LastName><ForeName>Ashok Kumar</ForeName><Initials>AK</Initials><AffiliationInfo><Affiliation>Analytical Research and Development, Aurex Laboratories LLC, 10 lake drive, East windsor, New Jersey 08520 USA.</Affiliation></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Katakam</LastName><ForeName>Lakshmi Narasimha Rao</ForeName><Initials>LNR</Initials><AffiliationInfo><Affiliation>Analytical Development, Saptalis Pharmaceuticals LLC, Hauppauge, NY 11788 USA.</Affiliation></AffiliationInfo></Author><Author ValidYN="Y"><LastName>Marisetti</LastName><ForeName>Vishnu Murthy</ForeName><Initials>VM</Initials><AffiliationInfo><Affiliation>Analytical Research and Development, ScieGen Pharmaceuticals Inc, 89 Arkay drive, Hauppauge, NY 11788 USA.</Affiliation></AffiliationInfo></Author></AuthorList><Language>eng</Language><PublicationTypeList><PublicationType UI="D016428">Journal Article</PublicationType></PublicationTypeList><ArticleDate DateType="Electronic"><Year>2020</Year><Month>08</Month><Day>25</Day></ArticleDate></Article><MedlineJournalInfo><Country>Germany</Country><MedlineTA>Chromatographia</MedlineTA><NlmUniqueID>0316520</NlmUniqueID><ISSNLinking>0009-5893</ISSNLinking></MedlineJournalInfo><KeywordList Owner="NOTNLM"><Keyword MajorTopicYN="N">Design of experiments</Keyword><Keyword MajorTopicYN="N">HPLC</Keyword><Keyword MajorTopicYN="N">Hydroxychloroquine sulfate</Keyword><Keyword MajorTopicYN="N">Quality by design</Keyword><Keyword MajorTopicYN="N">Validation</Keyword></KeywordList><CoiStatement>Conflict of InterestThe authors declare the absence of conflicts of interest.</CoiStatement></MedlineCitation><PubmedData><History><PubMedPubDate PubStatus="received"><Year>2020</Year><Month>03</Month><Day>03</Day></PubMedPubDate><PubMedPubDate PubStatus="revised"><Year>2020</Year><Month>07</Month><Day>18</Day></PubMedPubDate><PubMedPubDate PubStatus="accepted"><Year>2020</Year><Month>08</Month><Day>07</Day></PubMedPubDate><PubMedPubDate PubStatus="entrez"><Year>2020</Year><Month>9</Month><Day>1</Day><Hour>6</Hour><Minute>0</Minute></PubMedPubDate><PubMedPubDate PubStatus="pubmed"><Year>2020</Year><Month>8</Month><Day>31</Day><Hour>6</Hour><Minute>0</Minute></PubMedPubDate><PubMedPubDate PubStatus="medline"><Year>2020</Year><Month>8</Month><Day>31</Day><Hour>6</Hour><Minute>0</Minute></PubMedPubDate></History><PublicationStatus>aheadofprint</PublicationStatus><ArticleIdList><ArticleId IdType="pubmed">32863397</ArticleId><ArticleId IdType="doi">10.1007/s10337-020-03945-5</ArticleId><ArticleId IdType="pii">3945</ArticleId><ArticleId IdType="pmc">PMC7445446</ArticleId></ArticleIdList><pmc-dir>pmcsd</pmc-dir>
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