Detection of undeclared erectile dysfunction drugs and analogues in dietary supplements by ion mobility spectrometry
An ion mobility spectrometry (IMS) method was developed to screen for the presence of undeclared synthetic erectile dysfunction (ED) drugs or drug analogues in herbal dietary supplements claiming to enhance male sexual performance. Ion mobility spectra of authenticated reference materials including...
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| Veröffentlicht in: | Journal of pharmaceutical and biomedical analysis 2009-04, Vol.49 (3), p.601-606 |
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| container_title | Journal of pharmaceutical and biomedical analysis |
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| creator | Gryniewicz, Connie M. Reepmeyer, John C. Kauffman, John F. Buhse, Lucinda F. |
| description | An ion mobility spectrometry (IMS) method was developed to screen for the presence of undeclared synthetic erectile dysfunction (ED) drugs or drug analogues in herbal dietary supplements claiming to enhance male sexual performance. Ion mobility spectra of authenticated reference materials including three FDA approved drugs (sildenafil citrate, tadalafil, vardenafil hydrochloride trihydrate) and five previously identified synthetic analogues (methisosildenafil, homosildenafil, piperidenafil, thiosildenafil, thiomethisosildenafil) were measured to determine their reduced ion mobilities (K0). All eight compounds exhibited reduced mobilities between 0.8257 and 1.2876cm2/(Vs). Twenty-six herbal products were then screened for the presence of these compounds, and 15 of the 26 products tested positive for the presence of ED drug or drug analogue adulterants based on their reduced ion mobilities. IMS results were compared against the results obtained from an independent LC/MS reference method for the identical samples. Herbal dietary supplements containing adulterants were classified with 100% accuracy and most of the adulterants were correctly identified by a comparison of the K0 of the adulterant to the K0 of the authenticated reference material. The results demonstrate that IMS is a viable method for screening herbal dietary supplements for the presence of ED drug or drug analogue adulterants. |
| doi_str_mv | 10.1016/j.jpba.2008.12.002 |
| format | Article |
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Ion mobility spectra of authenticated reference materials including three FDA approved drugs (sildenafil citrate, tadalafil, vardenafil hydrochloride trihydrate) and five previously identified synthetic analogues (methisosildenafil, homosildenafil, piperidenafil, thiosildenafil, thiomethisosildenafil) were measured to determine their reduced ion mobilities (K0). All eight compounds exhibited reduced mobilities between 0.8257 and 1.2876cm2/(Vs). Twenty-six herbal products were then screened for the presence of these compounds, and 15 of the 26 products tested positive for the presence of ED drug or drug analogue adulterants based on their reduced ion mobilities. IMS results were compared against the results obtained from an independent LC/MS reference method for the identical samples. Herbal dietary supplements containing adulterants were classified with 100% accuracy and most of the adulterants were correctly identified by a comparison of the K0 of the adulterant to the K0 of the authenticated reference material. The results demonstrate that IMS is a viable method for screening herbal dietary supplements for the presence of ED drug or drug analogue adulterants.</description><identifier>ISSN: 0731-7085</identifier><identifier>EISSN: 1873-264X</identifier><identifier>DOI: 10.1016/j.jpba.2008.12.002</identifier><identifier>PMID: 19150190</identifier><identifier>CODEN: JPBADA</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Adult ; Adulterants ; Amines - analysis ; Analysis ; Analytical, structural and metabolic biochemistry ; Biological and medical sciences ; Carbolines - analysis ; Dietary Supplements - analysis ; Drug Contamination ; Erectile Dysfunction - drug therapy ; Erectile dysfunction drugs ; Fundamental and applied biological sciences. Psychology ; General pharmacology ; Herbal dietary supplements ; Humans ; Imidazoles - analysis ; Ion mobility spectrometry ; Ions - chemistry ; Male ; Medical sciences ; Pharmacology. Drug treatments ; Piperazines - analysis ; Plant Preparations - analysis ; Purines - analysis ; Reference Standards ; Sildenafil Citrate ; Spectrum Analysis ; Sulfones - analysis ; Tadalafil ; Triazines - analysis ; Vardenafil Dihydrochloride</subject><ispartof>Journal of pharmaceutical and biomedical analysis, 2009-04, Vol.49 (3), p.601-606</ispartof><rights>2008</rights><rights>2009 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c415t-8926d08e56b1064d352ceef046f36456e7bd3eb3cc39b620eb362970d7b9d76b3</citedby><cites>FETCH-LOGICAL-c415t-8926d08e56b1064d352ceef046f36456e7bd3eb3cc39b620eb362970d7b9d76b3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/j.jpba.2008.12.002$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,780,784,3550,27924,27925,45995</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=21289925$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/19150190$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Gryniewicz, Connie M.</creatorcontrib><creatorcontrib>Reepmeyer, John C.</creatorcontrib><creatorcontrib>Kauffman, John F.</creatorcontrib><creatorcontrib>Buhse, Lucinda F.</creatorcontrib><title>Detection of undeclared erectile dysfunction drugs and analogues in dietary supplements by ion mobility spectrometry</title><title>Journal of pharmaceutical and biomedical analysis</title><addtitle>J Pharm Biomed Anal</addtitle><description>An ion mobility spectrometry (IMS) method was developed to screen for the presence of undeclared synthetic erectile dysfunction (ED) drugs or drug analogues in herbal dietary supplements claiming to enhance male sexual performance. Ion mobility spectra of authenticated reference materials including three FDA approved drugs (sildenafil citrate, tadalafil, vardenafil hydrochloride trihydrate) and five previously identified synthetic analogues (methisosildenafil, homosildenafil, piperidenafil, thiosildenafil, thiomethisosildenafil) were measured to determine their reduced ion mobilities (K0). All eight compounds exhibited reduced mobilities between 0.8257 and 1.2876cm2/(Vs). Twenty-six herbal products were then screened for the presence of these compounds, and 15 of the 26 products tested positive for the presence of ED drug or drug analogue adulterants based on their reduced ion mobilities. IMS results were compared against the results obtained from an independent LC/MS reference method for the identical samples. Herbal dietary supplements containing adulterants were classified with 100% accuracy and most of the adulterants were correctly identified by a comparison of the K0 of the adulterant to the K0 of the authenticated reference material. The results demonstrate that IMS is a viable method for screening herbal dietary supplements for the presence of ED drug or drug analogue adulterants.</description><subject>Adult</subject><subject>Adulterants</subject><subject>Amines - analysis</subject><subject>Analysis</subject><subject>Analytical, structural and metabolic biochemistry</subject><subject>Biological and medical sciences</subject><subject>Carbolines - analysis</subject><subject>Dietary Supplements - analysis</subject><subject>Drug Contamination</subject><subject>Erectile Dysfunction - drug therapy</subject><subject>Erectile dysfunction drugs</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>General pharmacology</subject><subject>Herbal dietary supplements</subject><subject>Humans</subject><subject>Imidazoles - analysis</subject><subject>Ion mobility spectrometry</subject><subject>Ions - chemistry</subject><subject>Male</subject><subject>Medical sciences</subject><subject>Pharmacology. Drug treatments</subject><subject>Piperazines - analysis</subject><subject>Plant Preparations - analysis</subject><subject>Purines - analysis</subject><subject>Reference Standards</subject><subject>Sildenafil Citrate</subject><subject>Spectrum Analysis</subject><subject>Sulfones - analysis</subject><subject>Tadalafil</subject><subject>Triazines - analysis</subject><subject>Vardenafil Dihydrochloride</subject><issn>0731-7085</issn><issn>1873-264X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2009</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkUuLFDEUhYMoTs_oH3AhtdFdlTdJJVUBNzI6Kgy4UXAX8rg1pKmXSWqg_70putGdLkLCzXcOJzmEvKLQUKDy3bE5rtY0DKBvKGsA2BNyoH3Haybbn0_JATpO6w56cUWuUzoCgKCqfU6uqKICqIIDyR8xo8thmatlqLbZoxtNRF9h3McjVv6Uhm0-Iz5uD6kysy_LjMvDhqkKZRwwm3iq0rauI04451TZU7UrpsWGMeRytxa_uEyY4-kFeTaYMeHLy35Dftx9-n77pb7_9vnr7Yf72rVU5LpXTHroUUhLQbaeC-YQB2jlwGUrJHbWc7TcOa6sZFCOkqkOfGeV76TlN-Tt2XeNy6-SNespJIfjaGZctqRlB8DbXvwXZCC4aiUUkJ1BF5eUIg56jWEqb9cU9F6KPuq9FL2XoinTpZQien1x3-yE_q_k0kIB3lwAk5wZh2hmF9IfjlHWK8X2mO_PHJZPewwYdXIBZ4c-7G1pv4R_5fgN6wus2w</recordid><startdate>20090405</startdate><enddate>20090405</enddate><creator>Gryniewicz, Connie M.</creator><creator>Reepmeyer, John C.</creator><creator>Kauffman, John F.</creator><creator>Buhse, Lucinda F.</creator><general>Elsevier B.V</general><general>Elsevier</general><scope>IQODW</scope><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7U7</scope><scope>C1K</scope><scope>7X8</scope></search><sort><creationdate>20090405</creationdate><title>Detection of undeclared erectile dysfunction drugs and analogues in dietary supplements by ion mobility spectrometry</title><author>Gryniewicz, Connie M. ; Reepmeyer, John C. ; Kauffman, John F. ; Buhse, Lucinda F.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c415t-8926d08e56b1064d352ceef046f36456e7bd3eb3cc39b620eb362970d7b9d76b3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2009</creationdate><topic>Adult</topic><topic>Adulterants</topic><topic>Amines - analysis</topic><topic>Analysis</topic><topic>Analytical, structural and metabolic biochemistry</topic><topic>Biological and medical sciences</topic><topic>Carbolines - analysis</topic><topic>Dietary Supplements - analysis</topic><topic>Drug Contamination</topic><topic>Erectile Dysfunction - drug therapy</topic><topic>Erectile dysfunction drugs</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>General pharmacology</topic><topic>Herbal dietary supplements</topic><topic>Humans</topic><topic>Imidazoles - analysis</topic><topic>Ion mobility spectrometry</topic><topic>Ions - chemistry</topic><topic>Male</topic><topic>Medical sciences</topic><topic>Pharmacology. Drug treatments</topic><topic>Piperazines - analysis</topic><topic>Plant Preparations - analysis</topic><topic>Purines - analysis</topic><topic>Reference Standards</topic><topic>Sildenafil Citrate</topic><topic>Spectrum Analysis</topic><topic>Sulfones - analysis</topic><topic>Tadalafil</topic><topic>Triazines - analysis</topic><topic>Vardenafil Dihydrochloride</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Gryniewicz, Connie M.</creatorcontrib><creatorcontrib>Reepmeyer, John C.</creatorcontrib><creatorcontrib>Kauffman, John F.</creatorcontrib><creatorcontrib>Buhse, Lucinda F.</creatorcontrib><collection>Pascal-Francis</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>Toxicology Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><collection>MEDLINE - Academic</collection><jtitle>Journal of pharmaceutical and biomedical analysis</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Gryniewicz, Connie M.</au><au>Reepmeyer, John C.</au><au>Kauffman, John F.</au><au>Buhse, Lucinda F.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Detection of undeclared erectile dysfunction drugs and analogues in dietary supplements by ion mobility spectrometry</atitle><jtitle>Journal of pharmaceutical and biomedical analysis</jtitle><addtitle>J Pharm Biomed Anal</addtitle><date>2009-04-05</date><risdate>2009</risdate><volume>49</volume><issue>3</issue><spage>601</spage><epage>606</epage><pages>601-606</pages><issn>0731-7085</issn><eissn>1873-264X</eissn><coden>JPBADA</coden><abstract>An ion mobility spectrometry (IMS) method was developed to screen for the presence of undeclared synthetic erectile dysfunction (ED) drugs or drug analogues in herbal dietary supplements claiming to enhance male sexual performance. Ion mobility spectra of authenticated reference materials including three FDA approved drugs (sildenafil citrate, tadalafil, vardenafil hydrochloride trihydrate) and five previously identified synthetic analogues (methisosildenafil, homosildenafil, piperidenafil, thiosildenafil, thiomethisosildenafil) were measured to determine their reduced ion mobilities (K0). All eight compounds exhibited reduced mobilities between 0.8257 and 1.2876cm2/(Vs). Twenty-six herbal products were then screened for the presence of these compounds, and 15 of the 26 products tested positive for the presence of ED drug or drug analogue adulterants based on their reduced ion mobilities. IMS results were compared against the results obtained from an independent LC/MS reference method for the identical samples. Herbal dietary supplements containing adulterants were classified with 100% accuracy and most of the adulterants were correctly identified by a comparison of the K0 of the adulterant to the K0 of the authenticated reference material. The results demonstrate that IMS is a viable method for screening herbal dietary supplements for the presence of ED drug or drug analogue adulterants.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>19150190</pmid><doi>10.1016/j.jpba.2008.12.002</doi><tpages>6</tpages></addata></record> |
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| ispartof | Journal of pharmaceutical and biomedical analysis, 2009-04, Vol.49 (3), p.601-606 |
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| source | MEDLINE; Elsevier ScienceDirect Journals Complete |
| subjects | Adult Adulterants Amines - analysis Analysis Analytical, structural and metabolic biochemistry Biological and medical sciences Carbolines - analysis Dietary Supplements - analysis Drug Contamination Erectile Dysfunction - drug therapy Erectile dysfunction drugs Fundamental and applied biological sciences. Psychology General pharmacology Herbal dietary supplements Humans Imidazoles - analysis Ion mobility spectrometry Ions - chemistry Male Medical sciences Pharmacology. Drug treatments Piperazines - analysis Plant Preparations - analysis Purines - analysis Reference Standards Sildenafil Citrate Spectrum Analysis Sulfones - analysis Tadalafil Triazines - analysis Vardenafil Dihydrochloride |
| title | Detection of undeclared erectile dysfunction drugs and analogues in dietary supplements by ion mobility spectrometry |
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