Name: preparation of dmmtav and dmdtav using dmav for environmental applications: synthesis, purification, and confirmation
Uploaded: 2018-03-09T13:00:00
Description: Watch this Scientific Journal Video about Preparation of DMMTAV and DMDTAV Using DMAV for Environmental Applications: Synthesis, Purification, and Confirmation at JoVE.com

Denne forskningen ble støttet av grunnleggende forskning program (prosjektnummeret: 2016R1A2B4013467) gjennom de National Research Foundation av Korea (NRF) finansiert av departementet for vitenskap, IKT og fremtid planlegger 2016 og også støttet av Korea grunnleggende vitenskap Instituttet Research Program (prosjektnummeret: C36707).

1. syntese av DMMTAV
<ol><li>
Kjemisk forberedelse og molar forholdet blanding av DMAV, Na2S og H2SO4 Merk: DMAV: Na2S:H2så4 = 1:1.6:1.6<ol>
<li>Oppløse 5,24 g DMAV 40 mL vaskebuffer og N2-renset (slettet i minst 30 min) vann i et 50 mL sentrifuge rør.</li>
		<li>Klargjør Na2S reagens ved oppløsning 14.41 g Na2S·9H2O i 50 mL vaskebuffer og N<...

<ol>
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Toxicol. 24, 1586-1596 (2011).</li><li>Wallschlager, D., London, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Determination+of+methylated+arsenic-sulfur+compounds+in+groundwater.">Determination of methylated arsenic-sulfur compounds in groundwater.</a> Environ. Sci. Technol. 42, 228-234 (2008).</li><li>Zhang, J., Kim, H., Townsend, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Methodology+for+assessing+thioarsenic+formation+potential+in+sulfidic+landfill+environments.">Methodology for assessing thioarsenic formation potential in sulfidic landfill environments.</a> Chemosphere. 107, 311-318 (2014).</li><li>Shimoda, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Proposal+for+novel+metabolic+pathway+of+highly+toxic+dimethylated+arsenics+accompanied+by+enzymatic+sulfuration,+desulfuration+and+oxidation.">Proposal for novel metabolic pathway of highly toxic dimethylated arsenics accompanied by enzymatic sulfuration, desulfuration and oxidation.</a> Trace Elem. Med. Biol. 30, 129-136 (2015).</li><li>Naranmandura, H., Suzuki, T. 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D., Naranmandura, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Important+of+being+thiomethylated:+Formation,+Fate+and+Effects+of+methylated+thioarsenicals.">Important of being thiomethylated: Formation, Fate and Effects of methylated thioarsenicals.</a> Chem. Res. Toxicol. 25, 281-289 (2015).</li><li>Kim, Y. T., Lee, H., Yoon, H. O., Woo, N. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Kinetics+of+dimethylated+thioarsenicals+and+the+formation+of+highly+toxic+dimethylmonothioarsinic+acid+in+environment.">Kinetics of dimethylated thioarsenicals and the formation of highly toxic dimethylmonothioarsinic acid in environment.</a> Environ. Sci. Technol. 50, 11637-11645 (2016).</li><li>Cullen, W. R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Methylated+and+thiolated+arsenic+species+for+environmental+and+health+research+-+A+review+on+synthesis+and+characterization.">Methylated and thiolated arsenic species for environmental and health research - A review on synthesis and characterization.</a> J. Environ. Sci. 49, 7-27 (2016).</li><li>Fricke, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chromatographic+separation+and+identification+of+products+form+the+reaction+of+dimethylarsinic+acid+with+hydrogen+sulfide.">Chromatographic separation and identification of products form the reaction of dimethylarsinic acid with hydrogen sulfide.</a> Chem. Res. 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Pharmacol. 218, 166-173 (2007).</li><li>Jeong, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+of+a+simultaneous+analytical+method+to+determine+arsenic+speciation+using+HPLC-ICP-MS:+Arsenate,+arsenite,+monomethylarsonic+acid,+dimethylarsinic+acid,+dimethyldithioarsinic+acid,+and+dimethylmonothioarsinic+acid.">Development of a simultaneous analytical method to determine arsenic speciation using HPLC-ICP-MS: Arsenate, arsenite, monomethylarsonic acid, dimethylarsinic acid, dimethyldithioarsinic acid, and dimethylmonothioarsinic acid.</a> Microchem. J. 134, 295-300 (2017).</li><li>Li, Y., Low, C. -. K., Scott, A. J., Amal, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Arsenic+speciation+in+municipal+landfill+leachate.">Arsenic speciation in municipal landfill leachate.</a> Chemosphere. 79, 794-801 (2010).</li><li>Conklin, D. S., Fricke, W. M., Creed, A. P., Creed, J. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Investigation+of+the+pH+effects+on+the+formation+of+methylated+thio-arsenicals,+and+the+effects+of+pH+and+temperature+on+their+stability.">Investigation of the pH effects on the formation of methylated thio-arsenicals, and the effects of pH and temperature on their stability.</a> J. Anal. At. Spectrom. 23, 711-716 (2008).</li><li>Hansen, H. R., Raab, A., Jaspara, M., Milne, F. 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T., Anzai, K., Yamaguchi, K., Sei, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+SEC-HPLC-ICP-MS+hyphenated+technique+for+identification+of+sulfur-containing+arsenic+metabolites+in+biological+samples.">A SEC-HPLC-ICP-MS hyphenated technique for identification of sulfur-containing arsenic metabolites in biological samples.</a> J. Chromatogr. B. 874, 64-76 (2008).</li><li>Bartel, M., Ebert, F., Leffers, L., Karst, U., Schwerdtle, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Toxicological+characterization+of+the+inorganic+and+organic+arsenic+metabolite+thio-DMAV+in+cultured+human+lung+cells.">Toxicological characterization of the inorganic and organic arsenic metabolite thio-DMAV in cultured human lung cells.</a> J. 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Utviklet protokollen avklart avgjørende skritt at tidligere studier1,3,4,8,15 utelatt eller forkortet, som kan ha ført til problemer med eller feil under DMMTAV og DMDTAV syntese. DMMTAV er oksidasjon-sensitive1,5, kjemiske reagensene syntese dens ble tilberedt med N<...

Siden dimethylarsinic syre (DMAV) har vist seg å både Akutt toksisitet og gentoksisitet på grunn av gjennomgår metylering og thiolation ved svelging1,2, har metabolismevei av arsen thiolation er intensivt studerte både i vitro og vivo3,4 så vel som i environmental media (f.eks deponi sigevann)5,6. Tidligere studier har funnet både redusert og thiolated analogs av DMAV i levende celler, for eksempel, dimethylarsinous acid (DMAIII), dimethylmonothioarsinic syre (DMMTAV) og dimethyldithioarsinic syre ( DMDTAV)7,8,9, med dimethylated thioarsenicals som DMMTAV viser større toksisitet enn andre kjent uorganiske eller organiske arsenicals10. Overflod av svært giftige thioarsenicals har alvorlige miljømessige konsekvenser, siden de kan utgjøre en risiko for mennesker og miljø under svært sulfidic forhold11. Mekanismer for DMMTAV og DMDTAV (trans) dannelse og deres skjebne i miljømessige medier krever imidlertid fortsatt videre studier. Dermed kreves kvantitativ analyse av thioarsenicals for å bedre forståelsen av miljøkonsekvensene av DMMTAV og DMDTAV.
Selv om standard kjemikalier er viktig for kvantitativ analyse, standarder for DMMTAV og DMDTAV er vanskelig å få ved å replikere tidligere studier på grunn av høy risiko for arter transformasjon til andre arter og unstandardized syntese prosedyrer12. Dessuten har metodene referert begrensninger som kan føre til praktiske problemer i syntetisere standard kjemikalier og utføre kvantitativ analyse. DMMTAV og DMDTAV er vanligvis forberedt ved å blande DMAV, Na2S og H2så4 i en bestemt molar forholdet1 eller bobler H2S gass gjennom en løsning av DMAV 13,14. Boblende metoden funksjoner substitusjon av oksygen av svovel ved hjelp av en direkte levering av H2S gass, som er svært giftig og vanskelig å kontrollere for en uerfaren bruker. Derimot har over blande metoden1, brukte for kvalitativ analyse av DMMTAV og DMDTAV i miljømessig sudies5,6,12, thiolation av DMAV med H2S generert ved å blande Na2S og H2så4 og produserer DMMTAV og DMDTAV, gir enklere stoichiometric kontroll å produsere målet kjemikalier, som sammenlignet med direkte Bruk H2S gass.
Referansen blande metoden prosedyrer1,3,4,8,15 nevnt i denne studien utstillingen begrensninger i noen av sine kritiske eksperimentelle skritt, som kan føre til eksperimentell feil. For eksempel er informasjon om bestemte løsemiddel (dvs. vaskebuffer vann) forberedelse og utvinning og krystallisering av syntetisk arsenicals over forkortet eller ikke beskrevet i tilstrekkelig detalj. Slike spredt og begrenset informasjon om prosessuelle skritt kan føre til inkonsekvent dannelsen av thioarsenicals og upålitelige kvantifisering analyse. Derfor beskriver endret protokollen utviklet her syntese av DMMTAV og DMDTAV lager løsninger med kvantitative arter separasjon analyse.

<table width="712">
	<tbody>
		<tr height="21">
			<td height="21" style="width:179px;height:21px;">Cacodylic acid</td>
			<td style="width:179px;">Sigma-Aldrich</td>
			<td style="width:179px;">20835-10G-F</td>
			<td style="width:179px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="width:179px;height:42px;">Sodium sulfide nonahydrate</td>
			<td style="width:179px;">Sigma-Aldrich</td>
			<td style="width:179px;">S2006-500G</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="width:179px;height:21px;">Sulfuric acid 96%</td>
			<td style="width:179px;">J.T.Baker</td>
			<td style="width:179px;">0000011478</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="width:179px;height:21px;">Ammonium acetate</td>
			<td style="width:179px;">Sigma-Aldrich</td>
			<td style="width:179px;">A7262-500G</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="width:179px;height:42px;">Formic acid 98%</td>
			<td style="width:179px;">Wako Pure Chemical Industries, Ltd.</td>
			<td style="width:179px;">066-00461</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="width:179px;height:21px;">Diethyl ether (Extra Pure)</td>
			<td style="width:179px;">Junsei Chemical</td>
			<td style="width:179px;">33475-0380</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="width:179px;height:42px;">Adapter cap for 60 mL Bond Elut catridges</td>
			<td style="width:179px;">Agilent Technologies</td>
			<td style="width:179px;">12131004</td>
			<td>Syringe type of SPE</td>
		</tr>
		<tr height="21">
			<td height="21" style="width:179px;height:21px;">Bond Elut C18 cartridge</td>
			<td style="width:179px;">Agilent Technologies</td>
			<td style="width:179px;">14256031</td>
			<td>Syringe type of SPE</td>
		</tr>
		<tr height="21">
			<td height="21" style="width:179px;height:21px;">HyPURITY C-18</td>
			<td style="width:179px;">Thermo Scientific</td>
			<td style="width:179px;">22105-254630</td>
			<td>5 um, 125 x 4.6 mm</td>
		</tr>
		<tr height="42">
			<td height="42" style="width:179px;height:42px;">Glovebox</td>
			<td style="width:179px;">Chungae-chun, Rep. of Korea</td>
			<td style="width:179px;"></td>
			<td>Customized&#160;</td>
		</tr>
		<tr height="42">
			<td height="42" style="width:179px;height:42px;">Agilent 1260 Infinity Bio-inert LC</td>
			<td style="width:179px;">Agilent Technologies</td>
			<td style="width:179px;">DEAB600252, DEACH00245</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="width:179px;height:42px;">Agilent Technologies 7700 Series ICP-MS</td>
			<td style="width:179px;">Agilent Technologies</td>
			<td style="width:179px;">JP12031510</td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="width:179px;height:63px;">Finnigan LCQ Deca XP MAX Mass Spectrometer System</td>
			<td style="width:179px;">Thermo Electron Corporation</td>
			<td style="width:179px;">LDM10627</td>
			<td></td>
		</tr>
	</tbody>
</table>

preparation of dmmtav and dmdtav using dmav for environmental applications: synthesis, purification, and confirmation

Dimethylated thioarsenicals som dimethylmonothioarsinic syre (DMMTAV) og dimethyldithioarsinic syre (DMDTAV), som er produsert av metabolismevei av dimethylarsinic acid (DMAV) thiolation, har vært nylig funnet i miljø samt organer. DMMTAV og DMDTAV kan kvantifiseres for å fastslå økologiske effekter av dimethylated thioarsenicals og deres stabilitet i environmental media. Syntese metoden for disse forbindelsene er unstandardized, å replikere tidligere studier utfordrende. Videre er det en mangel på informasjon om lagring teknikker, inkludert lagring av forbindelser uten arter transformasjon. Videre begrenset informasjon om syntese metoder er tilgjengelig, kan det være eksperimentelle vanskeligheter med å syntetisere standard kjemikalier og utføre kvantitativ analyse. Protokollen presenteres her gir en praktisk endret syntese metode for dimethylated thioarsenicals, DMMTAV og DMDTAV, og vil hjelpe i kvantifiseringen arter separasjon analyse med høy ytelse flytende Ture i forbindelse med Induktivt kombinert plasma massespektrometri (såkalt HPLC-ICP-MS). Eksperimentell trinnene i denne fremgangsmåten ble endret ved å fokusere på utarbeidelsen av kjemiske reagenser, filtreringsmetoder og lagring.

Siden DMMTAV er feilaktig utarbeidet av DMAIII syntese metoden19, er verifikasjon av syntetisk DMMTAV og DMDTAV et kritisk punkt for syntese og utvinning og bestemme ideell standard kjemiske stoffer. Syntetiserte kjemikalier kan verifiseres av toppen av DMMTAV (MW 154 g·mol-1) og DMDTAV (MW 170 g·mol-1) masse-til-lade forholdet (m/z) bruke enten positive eller negativ...

Watch this Scientific Journal Video about Preparation of DMMTAV and DMDTAV Using DMAV for Environmental Applications: Synthesis, Purification, and Confirmation at JoVE.com

Preparation of DMMTAV and DMDTAV Using DMAV for Environmental Applications: Synthesis, Purification, and Confirmation

Utarbeidelse av DMMTAV og DMDTAV bruker DMAV for miljømessige programmer: syntese, rensing og bekreftelse

Denne artikkelen presenterer endret eksperimentelle protokoller for dimethylmonothioarsinic syre (DMMTAV) og dimethyldithioarsinic syre (DMDTAV) syntese, inducing dimethylarsinic syre (DMAV) thiolation gjennom blanding av DMAV , Na2S og H2så4. Endret protokollen inneholder en eksperimentell retningslinjer, dermed overvinne begrensninger av syntese trinnene som kan ha forårsaket eksperimentelle feil i kvantitativ analyse.

Dimethylated thioarsenicals such as dimethylmonothioarsinic acid (DMMTAV) and dimethyldithioarsinic acid (DMDTAV), which are produced by the metabolic ...

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Preparation of DMMTAV and DMDTAV Using DMAV for Environmental Applications: Synthesis, Purification, and Confirmation

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Using Caenorhabditis elegans for Studying Trans- and Multi-Generational Effects of Toxicants

Bruke Caenorhabditis elegans for å studere trans-og multi-generasjons effekter av toxicants

Information about toxicities of chemicals are essential in their application and waste management. For chemicals at low concentrations, the long-term ...

Studying Neurobehavioral Effects of Environmental Pollutants on Zebrafish Larvae

Studere neurobehavioral effekter av miljøforurensende stoffer på sebrafisk larver

Recent years more and more environmental pollutants have been proved neurotoxic, especially at the early development stages of organisms. Zebrafish larvae ...

Development and Testing of Species-specific Quantitative PCR Assays for Environmental DNA Applications

Utvikling og testing av artsspesifikke kvantitative PCR-analyser for miljø-DNA-applikasjoner

New, non-invasive methods for detecting and monitoring species presence are being developed to aid in fisheries and wildlife conservation management. The ...

Bioprospecting of Extremophilic Microorganisms to Address Environmental Pollution

Bioprospektering av extremofile mikroorganismer for å håndtere miljøforurensning

Geothermal springs are rich in various metal ions due to the interaction between rock and water that takes place in the deep aquifer. Moreover, due to ...