Determination of synephrine and octopamine in bitter orange peel by HPTLC with densitometry.
Identifieur interne : 001378 ( Ncbi/Merge ); précédent : 001377; suivant : 001379Determination of synephrine and octopamine in bitter orange peel by HPTLC with densitometry.
Auteurs : Eman Shawky [Oman]Source :
- Journal of chromatographic science [ 1945-239X ] ; 2014.
English descriptors
- KwdEn :
- MESH :
- chemical , analysis : Octopamine, Synephrine.
- chemistry : Citrus sinensis.
- methods : Chromatography, Thin Layer, Densitometry.
- Reproducibility of Results.
Abstract
This paper presents the development and validation of an improved method for the simultaneous analysis of synephrine and octopamine using high-performance thin-layer chromatography with densitometric detection. Separation was performed on silica gel 60F254 plates. The mobile phase is comprised of methanol, ethylacetate, methylene chloride and concentrated ammonia (2:2:1:0.05, v:v:v:v). The Rf values were 0.292 ± 0.0083 and 0.413 ± 0.0089 for synephrine and octopamine, respectively (n = 9). Ultraviolet absorbance detection at 277 nm was used for the alkaloids detection. Specificity, accuracy (recovery rates were between 96 and 99%) and precision (in both cases intra-day precision and inter-day precision were ≤ 2.0%) of the method were determined. Their amounts were calculated using the regression equations of the calibration curves which were linear in the range 0.2-1.2 µg/spot. The amounts of alkaloids in basic methanolic extracts of bitter orange peel measured by the method were 0.253 and 0.142% for synephrine and octopamine, respectively. Most of the factors evaluated in the robustness test were found to have an insignificant effect on the selected responses at 95% confidence level. The method was validated giving rise to a dependable and high-throughput procedure well suited to routine application.
DOI: 10.1093/chromsci/bmt113
PubMed: 23912767
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Separation was performed on silica gel 60F254 plates. The mobile phase is comprised of methanol, ethylacetate, methylene chloride and concentrated ammonia (2:2:1:0.05, v:v:v:v). The Rf values were 0.292 ± 0.0083 and 0.413 ± 0.0089 for synephrine and octopamine, respectively (n = 9). Ultraviolet absorbance detection at 277 nm was used for the alkaloids detection. Specificity, accuracy (recovery rates were between 96 and 99%) and precision (in both cases intra-day precision and inter-day precision were ≤ 2.0%) of the method were determined. Their amounts were calculated using the regression equations of the calibration curves which were linear in the range 0.2-1.2 µg/spot. The amounts of alkaloids in basic methanolic extracts of bitter orange peel measured by the method were 0.253 and 0.142% for synephrine and octopamine, respectively. Most of the factors evaluated in the robustness test were found to have an insignificant effect on the selected responses at 95% confidence level. The method was validated giving rise to a dependable and high-throughput procedure well suited to routine application.</div></front></TEI><pubmed><MedlineCitation Status="MEDLINE" Owner="NLM"><PMID Version="1">23912767</PMID><DateCreated><Year>2014</Year><Month>8</Month><Day>12</Day></DateCreated><DateCompleted><Year>2015</Year><Month>04</Month><Day>15</Day></DateCompleted><DateRevised><Year>2014</Year><Month>8</Month><Day>12</Day></DateRevised><Article PubModel="Print-Electronic"><Journal><ISSN IssnType="Electronic">1945-239X</ISSN><JournalIssue CitedMedium="Internet"><Volume>52</Volume><Issue>8</Issue><PubDate><Year>2014</Year><Month>Sep</Month></PubDate></JournalIssue><Title>Journal of chromatographic science</Title><ISOAbbreviation>J Chromatogr Sci</ISOAbbreviation></Journal><ArticleTitle>Determination of synephrine and octopamine in bitter orange peel by HPTLC with densitometry.</ArticleTitle><Pagination><MedlinePgn>899-904</MedlinePgn></Pagination><ELocationID EIdType="doi" ValidYN="Y">10.1093/chromsci/bmt113</ELocationID><Abstract><AbstractText>This paper presents the development and validation of an improved method for the simultaneous analysis of synephrine and octopamine using high-performance thin-layer chromatography with densitometric detection. Separation was performed on silica gel 60F254 plates. The mobile phase is comprised of methanol, ethylacetate, methylene chloride and concentrated ammonia (2:2:1:0.05, v:v:v:v). The Rf values were 0.292 ± 0.0083 and 0.413 ± 0.0089 for synephrine and octopamine, respectively (n = 9). Ultraviolet absorbance detection at 277 nm was used for the alkaloids detection. Specificity, accuracy (recovery rates were between 96 and 99%) and precision (in both cases intra-day precision and inter-day precision were ≤ 2.0%) of the method were determined. Their amounts were calculated using the regression equations of the calibration curves which were linear in the range 0.2-1.2 µg/spot. The amounts of alkaloids in basic methanolic extracts of bitter orange peel measured by the method were 0.253 and 0.142% for synephrine and octopamine, respectively. Most of the factors evaluated in the robustness test were found to have an insignificant effect on the selected responses at 95% confidence level. The method was validated giving rise to a dependable and high-throughput procedure well suited to routine application.</AbstractText><CopyrightInformation>© The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.</CopyrightInformation></Abstract><AuthorList CompleteYN="Y"><Author ValidYN="Y"><LastName>Shawky</LastName><ForeName>Eman</ForeName><Initials>E</Initials><AffiliationInfo><Affiliation>Faculty of Pharmacy, Department of Pharmacognosy, Alexandria University, Alkhartoom Square, Alexandria 21521, Egypt shawkyeman@yahoo.com.</Affiliation></AffiliationInfo></Author></AuthorList><Language>ENG</Language><PublicationTypeList><PublicationType UI="D016428">Journal Article</PublicationType></PublicationTypeList><ArticleDate DateType="Electronic"><Year>2013</Year><Month>Aug</Month><Day>02</Day></ArticleDate></Article><MedlineJournalInfo><Country>United States</Country><MedlineTA>J Chromatogr Sci</MedlineTA><NlmUniqueID>0173225</NlmUniqueID><ISSNLinking>0021-9665</ISSNLinking></MedlineJournalInfo><ChemicalList><Chemical><RegistryNumber>14O50WS8JD</RegistryNumber><NameOfSubstance UI="D009655">Octopamine</NameOfSubstance></Chemical><Chemical><RegistryNumber>PEG5DP7434</RegistryNumber><NameOfSubstance UI="D013578">Synephrine</NameOfSubstance></Chemical></ChemicalList><CitationSubset>IM</CitationSubset><MeshHeadingList><MeshHeading><DescriptorName UI="D002855" MajorTopicYN="N">Chromatography, Thin Layer</DescriptorName><QualifierName UI="Q000379" MajorTopicYN="Y">methods</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D032084" MajorTopicYN="N">Citrus sinensis</DescriptorName><QualifierName UI="Q000737" MajorTopicYN="Y">chemistry</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D003720" MajorTopicYN="N">Densitometry</DescriptorName><QualifierName UI="Q000379" MajorTopicYN="Y">methods</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D009655" MajorTopicYN="N">Octopamine</DescriptorName><QualifierName UI="Q000032" MajorTopicYN="Y">analysis</QualifierName></MeshHeading><MeshHeading><DescriptorName UI="D015203" MajorTopicYN="N">Reproducibility of Results</DescriptorName></MeshHeading><MeshHeading><DescriptorName UI="D013578" MajorTopicYN="N">Synephrine</DescriptorName><QualifierName UI="Q000032" MajorTopicYN="Y">analysis</QualifierName></MeshHeading></MeshHeadingList></MedlineCitation><PubmedData><History><PubMedPubDate PubStatus="entrez"><Year>2013</Year><Month>8</Month><Day>6</Day><Hour>6</Hour><Minute>0</Minute></PubMedPubDate><PubMedPubDate PubStatus="pubmed"><Year>2013</Year><Month>8</Month><Day>6</Day><Hour>6</Hour><Minute>0</Minute></PubMedPubDate><PubMedPubDate PubStatus="medline"><Year>2015</Year><Month>4</Month><Day>16</Day><Hour>6</Hour><Minute>0</Minute></PubMedPubDate></History><PublicationStatus>ppublish</PublicationStatus><ArticleIdList><ArticleId IdType="pubmed">23912767</ArticleId><ArticleId IdType="pii">bmt113</ArticleId><ArticleId IdType="doi">10.1093/chromsci/bmt113</ArticleId></ArticleIdList></PubmedData></pubmed><affiliations><list><country><li>Oman</li></country></list><tree><country name="Oman"><noRegion><name sortKey="Shawky, Eman" sort="Shawky, Eman" uniqKey="Shawky E" first="Eman" last="Shawky">Eman Shawky</name></noRegion></country></tree></affiliations></record>Pour manipuler ce document sous Unix (Dilib)
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