Stability-indicating high performance thin layer chromatographic determination of sulfanilamide in human urine
A simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic ( HPTLC ) method was developed and applied to human urine for the densitometric determination of sulfanilamide. A mixture of chloroform-ethyl acetate-xylene (2.5: 4.0: 1.0, v/v/v) was used as...
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Veröffentlicht in: | Journal of analytical chemistry (New York, N.Y.) N.Y.), 2009-07, Vol.64 (7), p.714-720 |
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creator | Kilinc, E. Gumgum, B. Hamamci, C. Aydin, F. |
description | A simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (
HPTLC
) method was developed and applied to human urine for the densitometric determination of sulfanilamide. A mixture of chloroform-ethyl acetate-xylene (2.5: 4.0: 1.0, v/v/v) was used as a mobile phase. The system was found to give compact spots for sulfanilamide (retardation factor,
R
f
= 0.21±0.02). The linear regression analysis data for the calibration plots showed good linear relationship with
r
2
= 0.9970 ± 0.0003 and
r
2
= 0.9947 ± 0.020 within the concentration range of 50–250 ng per spot and 100–1000 ng per spot with respect to peak area, respectively. The limit of detection (
LOD
) and quantification (
LOQ
) were 8 and 25 ng per spot, respectively. Sulfanilamide was subjected to acid and alkali hydrolysis, oxidation, dry heat and wet heat treatment. According to the International Conference on Harmonization (
ICH
) guidelines the method was validated for precision, recovery and robustness. The ultraviolet (
UV
) spectra of the degradation products which had different spectra from sulfanilamide were also recorded. |
doi_str_mv | 10.1134/S1061934809070090 |
format | Article |
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HPTLC
) method was developed and applied to human urine for the densitometric determination of sulfanilamide. A mixture of chloroform-ethyl acetate-xylene (2.5: 4.0: 1.0, v/v/v) was used as a mobile phase. The system was found to give compact spots for sulfanilamide (retardation factor,
R
f
= 0.21±0.02). The linear regression analysis data for the calibration plots showed good linear relationship with
r
2
= 0.9970 ± 0.0003 and
r
2
= 0.9947 ± 0.020 within the concentration range of 50–250 ng per spot and 100–1000 ng per spot with respect to peak area, respectively. The limit of detection (
LOD
) and quantification (
LOQ
) were 8 and 25 ng per spot, respectively. Sulfanilamide was subjected to acid and alkali hydrolysis, oxidation, dry heat and wet heat treatment. According to the International Conference on Harmonization (
ICH
) guidelines the method was validated for precision, recovery and robustness. The ultraviolet (
UV
) spectra of the degradation products which had different spectra from sulfanilamide were also recorded.</description><identifier>ISSN: 1061-9348</identifier><identifier>EISSN: 1608-3199</identifier><identifier>DOI: 10.1134/S1061934809070090</identifier><language>eng</language><publisher>Dordrecht: SP MAIK Nauka/Interperiodica</publisher><subject>Analytical Chemistry ; Chemistry ; Chemistry and Materials Science</subject><ispartof>Journal of analytical chemistry (New York, N.Y.), 2009-07, Vol.64 (7), p.714-720</ispartof><rights>Pleiades Publishing, Ltd. 2009</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c288t-4aef1f5c54a04738d0dcb5d05614a4eef64895e8efe325753325e2ae63e855883</citedby><cites>FETCH-LOGICAL-c288t-4aef1f5c54a04738d0dcb5d05614a4eef64895e8efe325753325e2ae63e855883</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://link.springer.com/content/pdf/10.1134/S1061934809070090$$EPDF$$P50$$Gspringer$$H</linktopdf><linktohtml>$$Uhttps://link.springer.com/10.1134/S1061934809070090$$EHTML$$P50$$Gspringer$$H</linktohtml><link.rule.ids>314,780,784,27924,27925,41488,42557,51319</link.rule.ids></links><search><creatorcontrib>Kilinc, E.</creatorcontrib><creatorcontrib>Gumgum, B.</creatorcontrib><creatorcontrib>Hamamci, C.</creatorcontrib><creatorcontrib>Aydin, F.</creatorcontrib><title>Stability-indicating high performance thin layer chromatographic determination of sulfanilamide in human urine</title><title>Journal of analytical chemistry (New York, N.Y.)</title><addtitle>J Anal Chem</addtitle><description>A simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (
HPTLC
) method was developed and applied to human urine for the densitometric determination of sulfanilamide. A mixture of chloroform-ethyl acetate-xylene (2.5: 4.0: 1.0, v/v/v) was used as a mobile phase. The system was found to give compact spots for sulfanilamide (retardation factor,
R
f
= 0.21±0.02). The linear regression analysis data for the calibration plots showed good linear relationship with
r
2
= 0.9970 ± 0.0003 and
r
2
= 0.9947 ± 0.020 within the concentration range of 50–250 ng per spot and 100–1000 ng per spot with respect to peak area, respectively. The limit of detection (
LOD
) and quantification (
LOQ
) were 8 and 25 ng per spot, respectively. Sulfanilamide was subjected to acid and alkali hydrolysis, oxidation, dry heat and wet heat treatment. According to the International Conference on Harmonization (
ICH
) guidelines the method was validated for precision, recovery and robustness. The ultraviolet (
UV
) spectra of the degradation products which had different spectra from sulfanilamide were also recorded.</description><subject>Analytical Chemistry</subject><subject>Chemistry</subject><subject>Chemistry and Materials Science</subject><issn>1061-9348</issn><issn>1608-3199</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2009</creationdate><recordtype>article</recordtype><recordid>eNp9kM1qwzAQhEVpoWnaB-hNL-BWsiRHPpbQPwj0kPZsNvLKVrDlIMmHvH0V0lshl9mFnW9YhpBHzp44F_J5y1nFayE1q9mKZbkiC14xXQhe19d5z-fidL8ldzHuWbZoXi2I3ybYucGlY-F86wwk5zvau66nBwx2CiN4gzT1ztMBjhio6cM0Qpq6AIfeGdpiwjA6n8nJ08nSOA8WvBtgdC3SzPVzDqFzcB7vyY2FIeLD31ySn7fX7_VHsfl6_1y_bApTap0KCWi5VUZJYHIldMtas1MtUxWXIBFtJXWtUKNFUaqVElmxBKwEaqW0FkvCz7kmTDEGtM0huBHCseGsORXW_CssM-WZidnrOwzNfpqDz29egH4Bywlvww</recordid><startdate>20090701</startdate><enddate>20090701</enddate><creator>Kilinc, E.</creator><creator>Gumgum, B.</creator><creator>Hamamci, C.</creator><creator>Aydin, F.</creator><general>SP MAIK Nauka/Interperiodica</general><scope>AAYXX</scope><scope>CITATION</scope></search><sort><creationdate>20090701</creationdate><title>Stability-indicating high performance thin layer chromatographic determination of sulfanilamide in human urine</title><author>Kilinc, E. ; Gumgum, B. ; Hamamci, C. ; Aydin, F.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c288t-4aef1f5c54a04738d0dcb5d05614a4eef64895e8efe325753325e2ae63e855883</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2009</creationdate><topic>Analytical Chemistry</topic><topic>Chemistry</topic><topic>Chemistry and Materials Science</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Kilinc, E.</creatorcontrib><creatorcontrib>Gumgum, B.</creatorcontrib><creatorcontrib>Hamamci, C.</creatorcontrib><creatorcontrib>Aydin, F.</creatorcontrib><collection>CrossRef</collection><jtitle>Journal of analytical chemistry (New York, N.Y.)</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Kilinc, E.</au><au>Gumgum, B.</au><au>Hamamci, C.</au><au>Aydin, F.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Stability-indicating high performance thin layer chromatographic determination of sulfanilamide in human urine</atitle><jtitle>Journal of analytical chemistry (New York, N.Y.)</jtitle><stitle>J Anal Chem</stitle><date>2009-07-01</date><risdate>2009</risdate><volume>64</volume><issue>7</issue><spage>714</spage><epage>720</epage><pages>714-720</pages><issn>1061-9348</issn><eissn>1608-3199</eissn><abstract>A simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (
HPTLC
) method was developed and applied to human urine for the densitometric determination of sulfanilamide. A mixture of chloroform-ethyl acetate-xylene (2.5: 4.0: 1.0, v/v/v) was used as a mobile phase. The system was found to give compact spots for sulfanilamide (retardation factor,
R
f
= 0.21±0.02). The linear regression analysis data for the calibration plots showed good linear relationship with
r
2
= 0.9970 ± 0.0003 and
r
2
= 0.9947 ± 0.020 within the concentration range of 50–250 ng per spot and 100–1000 ng per spot with respect to peak area, respectively. The limit of detection (
LOD
) and quantification (
LOQ
) were 8 and 25 ng per spot, respectively. Sulfanilamide was subjected to acid and alkali hydrolysis, oxidation, dry heat and wet heat treatment. According to the International Conference on Harmonization (
ICH
) guidelines the method was validated for precision, recovery and robustness. The ultraviolet (
UV
) spectra of the degradation products which had different spectra from sulfanilamide were also recorded.</abstract><cop>Dordrecht</cop><pub>SP MAIK Nauka/Interperiodica</pub><doi>10.1134/S1061934809070090</doi><tpages>7</tpages></addata></record> |
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issn | 1061-9348 1608-3199 |
language | eng |
recordid | cdi_crossref_primary_10_1134_S1061934809070090 |
source | SpringerNature Journals |
subjects | Analytical Chemistry Chemistry Chemistry and Materials Science |
title | Stability-indicating high performance thin layer chromatographic determination of sulfanilamide in human urine |
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