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 forskning blev støttet af grundlæggende videnskabsforskning program (projekt nummer: 2016R1A2B4013467) gennem National Research Foundation af Korea (NRF) finansieret af Ministeriet for videnskab, IKT & fremtid planlægning 2016 og også støttet af Korea grundlæggende videnskab Institut Research Program (projekt nummer: C36707).

1. Sammenfatning af DMMTAV
<ol><li>
Kemiske forberedelse og molære forhold blanding af DMAV, Na2S og H2SO4 Bemærk: DMAV: Na2S:H2så4 = 1:1.6:1.6<ol>
<li>Opløse 5,24 g af DMAV i 40 mL deioniseret vand og N2-renset (renset for mindst 30 min.) vand i en 50 mL-centrifugerør.</li>
		<li>Forberede Na2S reagens ved at opløse 14.41 g Na2S·9H2O i 50 m...

<ol>
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T., Ogra, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Distribution+and+metabolism+of+four+different+dimethylated+arsenicals+in+hamsters.">Distribution and metabolism of four different dimethylated arsenicals in hamsters.</a> Toxicol. Appl. Pharmacol. 245, 67-75 (2010).</li><li>Naranmandura, H., 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=Comparative+toxicity+of+arsenic+metabolites+in+human+bladder+cancer+EJ-1+cells.">Comparative toxicity of arsenic metabolites in human bladder cancer EJ-1 cells.</a> Chem. Res. 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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Udviklede protokollen har afklaret kritiske trin at tidligere undersøgelser1,3,4,8,15 udeladt eller forkortet, kan som har ført til vanskeligheder med eller svigt under DMMTAV og DMDTAV syntese. Da DMMTAV oxidation-følsomme1,5, kemiske reagenser til sin syntese blev ...

Da dimethylarsinic syre (DMAV) er blevet påvist for at udstille både akutte toksicitet og genotoksicitet på grund af gennemgår methylering og thiolation ved indtagelse1,2, har stofskiftevej af arsen thiolation været intensivt undersøgt både in vitro- og i vivo3,4 såvel som i miljømedier (f.eks. lossepladser perkolat)5,6. Tidligere undersøgelser har fundet både reduceret og thiolated analoger af DMAV i levende celler, for eksempel, dimethylarsinous syre (DMAIII), dimethylmonothioarsinic syre (DMMTAV) og dimethyldithioarsinic syre ( DMDTAV)7,8,9, med dimethylated thioarsenicals som DMMTAV udviser større toksicitet end andre kendte uorganiske eller organiske arsenicals10. Overfloden af meget giftige thioarsenicals har alvorlige miljømæssige konsekvenser, da de kan udgøre en risiko for mennesker og miljø under meget kun sker betingelser11. Mekanismerne i DMMTAV og DMDTAV (trans) dannelse og deres skæbner i miljømedierne kræver dog stadig yderligere undersøgelse. Således, kvantitativ analyse af thioarsenicals er forpligtet til at forbedre forståelsen af de miljømæssige virkninger af DMMTAV og DMDTAV.
Selv om standard kemikalier er det centrale krav til kvantitativ analyse, standarder for DMMTAV og DMDTAV er vanskelig at opnå ved at gentage tidligere undersøgelser, på grund af den høje risiko for arter omdannelse til andre arter og unstandardized syntese procedurer12. Derudover har metoderne refereres til begrænsninger, der kan føre til praktiske vanskeligheder i syntese af standard kemikalier og udfører kvantitativ analyse. DMMTAV og DMDTAV er almindeligvis fremstilles ved at blande DMAV, Na2S og H2så4 i en visse molære forhold1 eller boblende H2S gas gennem en løsning af DMAV 13,14. Den boblende metode funktioner substitution af ilt af svovl ved hjælp af en direkte levering af H2S gas, som er yderst giftigt og svært at kontrollere for en uerfaren bruger. Omvendt er har den ovennævnte blanding metode1, udbredte til kvalitativ analyse af DMMTAV og DMDTAV i miljømæssige sudies5,6,12, thiolation af DMAV med H2S genereret ved at blande Na2S og H2så4 og producerer DMMTAV og DMDTAV, så lettere støkiometriske kontrol til at producere mål kemikalier, som i forhold til direkte Brug af H-gas og2S.
Referencen blanding metode procedurer1,3,4,8,15 nævnt i denne undersøgelse udstille begrænsninger i nogle af deres kritiske eksperimenterende trin, som kan føre til Eksperimentel fejl. For eksempel er oplysninger om specifikke opløsningsmiddel (dvs., deioniseret vand) forberedelse og ekstraktion og krystallisering af de syntetiserede arsenicals over forkortet eller ikke beskrevet tilstrækkelig detaljeret. Sådan spredt og begrænsede oplysninger om proceduremæssige skridt kan føre til usammenhængende dannelsen af thioarsenicals og upålidelige kvantificering analyse. Den ændrede protokol udviklet Heri beskrives derfor, syntesen af DMMTAV og DMDTAV stamopløsninger med kvantitative arter adskillelse 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 produceret af stofskiftevej af dimethylarsinic syre (DMAV) thiolation, har været for nylig fundet i miljøet samt menneskelige organer. DMMTAV og DMDTAV kan kvantificeres for at bestemme de økologiske virkninger af dimethylated thioarsenicals og deres stabilitet i miljømedierne. Metoden syntese for disse forbindelser er unstandardized, at gentage tidligere undersøgelser udfordrende. Derudover mangler information om opbevaring teknikker, herunder opbevaring af forbindelser uden arter transformation. Desuden, fordi kun begrænsede oplysninger om syntese metoder er tilgængelige, kan der være eksperimenterende vanskeligheder i syntese standard kemikalier og udfører kvantitativ analyse. Protokollen præsenteres heri giver en praktisk modificerede syntese metode for dimethylated thioarsenicals, DMMTAV og DMDTAV, og vil hjælpe med kvantificeringen af arter adskillelse analyse ved hjælp af højtydende væske kromatografi sammenholdt med Induktivt koblet plasma massespektrometri (HPLC-ICP-MS). De eksperimenterende trin i denne procedure blev ændret ved at fokusere på udarbejdelsen af kemiske reagenser, filtrering metoder og opbevaring.

Da DMMTAV er udarbejdet fejlagtigt af DMAIII syntese metode19, er verifikation af syntetiserede DMMTAV og DMDTAV et afgørende skridt til syntese og ekstraktion og bestemmelse af den ideelle standard kemiske materialer. Syntetiserede kemikalier kan verificeres ved peak af DMMTAV (MW 154 g·mol-1) og DMDTAV (MW 170 g·mol-1) masse til ladning forhold (m/z) ved hjælp af ...

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

Forberedelse af DMMTAV og DMDTAV bruger DMAV for miljømæssige programmer: syntese, rensning og bekræftelse

Denne artikel præsenterer modificerede eksperimentelle protokoller til dimethylmonothioarsinic syre (DMMTAV) og dimethyldithioarsinic syre (DMDTAV) syntese, inducerende dimethylarsinic syre (DMAV) thiolation gennem blanding af DMAV , Na2S og H2så4. Den ændrede protokol giver en eksperimentel retningslinje, derved at overvinde begrænsninger af trinene syntese, der kunne have forårsaget eksperimentelle fejl 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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Long-term studies enable the identification of eco-evolutionary processes that occur over extended time periods. In addition, they provide key empirical ...

Composition and Distribution Analysis of Bioaerosols Under Different Environmental Conditions

Sammensætning og Distribution analyse af Bioaerosols Under forskellige miljøforhold

Variable microorganisms in particulate matter (PM) under different environmental conditions may have significant impacts on human health. In this study, ...

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

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

Brug af Caenorhabditis elegans til at studere Trans-og multi generations effekter af giftstoffer

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

Undersøgelse Neurobehavioral Virkninger af miljøforurenende stoffer på Zebrafisk 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

Udvikling og afprøvning af artsspecifikke kvantitative PCR-analyser til miljø-DNA-applikationer

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 af ekstremofile mikroorganismer til bekæmpelse af miljøforurening

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 ...