Name: fizzy extraction of volatile organic compounds combined with atmospheric pressure chemical ionization quadrupole mass spectrometry
Uploaded: 2017-07-14T13:00:00
Description: Watch this Scientific Journal Video about Fizzy Extraction of Volatile Organic Compounds Combined with Atmospheric Pressure Chemical Ionization Quadrupole Mass Spectrometry at JoVE.com

Vi vil gjerne takke Vitenskapsdepartementet i Taiwan (bevilgningsnummer: MOST 104-2628-M-009-003-MY4) for økonomisk støtte til dette arbeidet.

Denne protokollen forutsetter at alle trinnene utføres i samsvar med de relevante laboratorieforskrifter. Noen av trinnene bruker kommersielle instrumenter - i slike tilfeller må produsentens retningslinjer følges. Ved håndtering av giftige kjemikalier må retningslinjer for helsedirektorater følges. Det spesialtilpassede utstyret 4 må betjenes forsiktig; Spesielt når man håndterer trykkgasser og lever elektrisk ledninger. 1. Fremstilling av standardløsning </p...

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N., Horning, M. G., Horning, E. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Subpicogram+detection+system+for+gas+phase+analysis+based+upon+atmospheric+pressure+ionization+(API)+mass+spectrometry.">Subpicogram detection system for gas phase analysis based upon atmospheric pressure ionization (API) mass spectrometry.</a> Anal Chem. 46, 706-710 (1974).</li><li>Carroll, D. I., Dzidic, I., Stillwell, R. N., Haegele, K. D., Horning, E. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atmospheric+pressure+ionization+mass+spectrometry.+Corona+discharge+ion+source+for+use+in+a+liquid+chromatograph-mass+spectrometer-computer+analytical+system.">Atmospheric pressure ionization mass spectrometry. Corona discharge ion source for use in a liquid chromatograph-mass spectrometer-computer analytical system.</a> Anal Chem. 47, 2369-2373 (1975).</li><li>Hakim, I. A., McClure, T., Liebler, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Assessing+dietary+D-limonene+intake+for+epidemiological+studies.">Assessing dietary D-limonene intake for epidemiological studies.</a> J Food Compos Anal. 13, 329-336 (2000).</li></ol>

<html> Flere klare måter å levere prøver til et massespektrometer ble utviklet i de studier som ble utført i løpet av de siste tre tiårene ( f.eks . Referanser 8 , 9 , 10 , 11 , 12 , 13 , 14 ). Et av målene med disse studiene var å forenkle forberedelsen av prøver til analy...

Forskjellige fenomener som observeres i naturen og dagliglivet, er knyttet til gass-væskefase-likevekt. Kullsyre er oppløst i myke og alkoholholdige drikker under forhøyet trykk. Når en flaske med en så myk drikk åpnes, faller trykket ned, og gassbobler rush til væskeoverflaten. I dette tilfellet forbedrer bruddet organoleptiske egenskaper til drikkevarer. Utgivelsen av gassbobler er også hovedårsaken til dekompresjonssyke (&quot;bøyene&quot;) 1 . På grunn av plutselig dekompresjon dannes bobler i dykkers kropp. Personer som lider av dekompresjonssyke, blir behandlet i hyperbariske kamre. Gassbobler har forskjellige anvendelser i analytisk kjemi. Spesielt sprer metoder for å overføre gassbobler gjennom flytende prøver for å ekstrahere flyktige forbindelser 2 . For eksempel kombineres en metode som kalles &quot;purge-closed loop&quot; med gaskromatografi for å muliggjøre rask analyse av diSosolved flyktige stoffer 3 . Mens sparging kontinuerlig kan trekke ut flyktige stoffer over tid, begrenser det ikke dem i rom eller tid. Den frigjorte gassfase-arten må fanges, og i noen tilfeller-konsentrert ved å anvende et temperaturprogram eller ved hjelp av sorbenter. Dermed er det behov for å introdusere nye on-line prøvebehandlingsstrategier, som kan redusere antall trinn, og samtidig konsentrere volatile analytter i rom eller tid. For å løse utfordringen med å utvinne flyktige forbindelser fra flytende prøver og utføre analyse på nettet, introduserte vi nylig &quot;fizzy extraction&quot; 4 . Denne nye teknikken utnytter bruksfenomenet. I korte trekk oppløses en bærer gass (her karbondioksyd) først i prøven ved å påføre overtrykk og omrøre prøven. Så dekomprimeres prøvekammeret brått. Den plutselige dekompresjonen fører til dannelse av en rekke bærergassbobler<html> I prøvevæsken. Disse boblene hjelper frigjøringen av oppløste analytter fra væsken til gassfasen. De frigjorte analysene overføres umiddelbart til massespektrometeret, som produserer signaler i tidsdomene. Fordi frigjøringen av analysetypen er begrenset til kort tid (noen få sekunder), har de tidsmessige signalene høye amplituder og høye signal-til-støyforhold. Trykket involvert i mykekstraksjonsprosessen er svært lavt (~ 150 kPa) 4 ; Mye lavere enn i superkritisk fluidutvinning 5 ( f.eks . ≥10 MPa). Teknikken krever ikke bruk av spesielle forbruksvarer (kolonner, patroner). Bare små mengder løsningsmidler brukes til fortynning og rengjøring. Ekstraksjonsanordningen kan settes sammen av kjemikere med middels tekniske ferdigheter ved å bruke allment tilgjengelige deler 4 ; For eksempel elektroniske moduler med åpen kildekode&quot;&gt; 6 , 7. Fizzy-ekstraksjon kan kobles på nettet med moderne massespektrometre utstyrt med APCI-grensesnitt. I tillegg til at gassfaseekstrakter overføres til ionkilden, påvirker driften av mykekstraksjonen ikke vesentlig sårbar Deler av massespektrometeret. Formålet med denne visualiserte eksperimentartikkelen er å veilede seerne om hvordan man implementerer mykekstraksjon i en enkel analytisk oppgave. Mens kjernen i mykekstraksjonssystemet er som beskrevet i vår tidligere rapport 4 , har flere forbedringer blitt innført for å gjøre operasjonen mer enkel. En mikrokontroller utstyrt med en LCD-skjerm skjerm er blitt innlemmet i systemet for å vise nøkkelutvinningsparametrene i sanntid. Alle funksjonene er programmert i microcontroller-skriptene, og det er ikke lenger nødvendig å bruke en ekstern datamaskin til cAvtrekk uttrekkssystemet.

<table border="0" cellpadding="0" cellspacing="0" width="963">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">Water</td>
			<td style="width:197px;">Fisher</td>
			<td style="width:160px;">W6212</td>
			<td style="width:191px;">Diluent</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">Ethanol</td>
			<td style="width:197px;">Sigma-Aldrich</td>
			<td style="width:160px;">32221-2.5L</td>
			<td>Diluent</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">(R)-(+)-Limonene</td>
			<td style="width:197px;">Sigma-Aldrich</td>
			<td style="width:160px;">183164-100ML</td>
			<td>Standard</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">Carbon dioxide</td>
			<td style="width:197px;">ChiaLung</td>
			<td>n/a</td>
			<td>Carrier gas</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">Cellulose tissue, Kimwipes Kimtech</td>
			<td style="width:197px;">Kimberly-Clark</td>
			<td>34120</td>
			<td>Used for cleaning</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">Triple quadrupole mass spectrometer</td>
			<td style="width:197px;">Shimadzu</td>
			<td style="width:160px;">LCMS-8030</td>
			<td>Detection system</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">Atmospheric pressure chemical ionization interface</td>
			<td style="width:197px;">Shimadzu</td>
			<td style="width:160px;">Duis</td>
			<td>Ion source</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">20-mL screw top headspace glass vial with septum cap</td>
			<td style="width:197px;">Thermo Fisher Scientific</td>
			<td style="width:160px;">D-52379</td>
			<td>Sample vial</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">LabSolutions software</td>
			<td style="width:197px;">Shimadzu</td>
			<td>n/a</td>
			<td>version 5.82</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">PeakFit software</td>
			<td style="width:197px;">Systat Software</td>
			<td>n/a</td>
			<td>version 4.12</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:415px;">OriginPro software</td>
			<td style="width:197px;">OriginLab</td>
			<td>n/a</td>
			<td>version 8</td>
		</tr>
	</tbody>
</table>

fizzy extraction of volatile organic compounds combined with atmospheric pressure chemical ionization quadrupole mass spectrometry

Kjemisk analyse av flyktige og semivolatile forbindelser oppløst i flytende prøver kan være utfordrende. De oppløste komponentene må bringes til gassfasen og overføres effektivt til et deteksjonssystem. Fizzy ekstraksjon utnytter brennbarhetsfenomenet. Først oppløses en bærer gass (her karbondioksyd) i prøven ved å påføre overtrykk og omrøre prøven. For det andre dekomprimeres prøvekammeret brått. Dekompresjon fører til dannelsen av en rekke bærergassbobler i prøvevæsken. Disse boblene hjelper frigjøringen av den oppløste analytten fra væsken til gassfasen. De frigjorte analyttene overføres umiddelbart til det kjemiske ioniseringsgrensesnittet for atmosfærisk trykk av et triple quadrupole massespektrometer. Den ioniserbare analyserte arten gir opphav til massespektrometriske signaler i tidsdomene. Fordi frigjøringen av analytartene skjer over korte tidsperioder (noen få sekunderOnds), de tidsmessige signalene har høye amplituder og høye signal-til-støy-forhold. Amplitudene og områdene av de temporale topper kan da korreleres med konsentrasjoner av analyttene i væskeprøvene utsatt for sopputvinning, som muliggjør kvantitativ analyse. Fordelene med mykekstraksjon inkluderer: enkelhet, fart og begrenset bruk av kjemikalier (løsningsmidler).

I begynnelsen testes fizzy-ekstraksjonssystemet med en standardløsning. Deretter analyseres den virkelige prøven og den virkelige prøven med standard. Arealene av de tidlige toppene av utvinningshendelser er korrelert med konsentrasjoner av analyttene i væskeprøvene utsatt for sopputvinning, som muliggjør kvantitativ analyse. Her har vi utført dobbelt standard tillegg for å demonstrere kvantitative evner av teknikken ( Figur 7 ). Den lineære regresj...

Watch this Scientific Journal Video about Fizzy Extraction of Volatile Organic Compounds Combined with Atmospheric Pressure Chemical Ionization Quadrupole Mass Spectrometry at JoVE.com

Fizzy Extraction of Volatile Organic Compounds Combined with Atmospheric Pressure Chemical Ionization Quadrupole Mass Spectrometry

Fizzy extraction er en ny laboratorieteknikk for analyse av flyktige og semivolatile forbindelser. En bærer gass oppløses i væskeprøven ved å påføre overtrykk og omrøre prøven. Prøvekammeret dekomprimeres deretter. Analyttens art frigjøres til gassfasen på grunn av brudd.

Fizzy Ekstraksjon av flyktige organiske forbindelser kombinert med atmosfærisk trykk kjemisk ionisering Quadrupole massespektrometri

Chemical analysis of volatile and semivolatile compounds dissolved in liquid samples can be challenging. The dissolved components need to be brought to ...

The overall goal of this extraction procedure is to liberate volatile compounds from a liquid sample and to transfer these compounds to the mass spectrometer for detection. This method can help answer key questions in the field of science or environmental chemistry field such as what volatile compounds are present in beverages or waste water. The main advantage of this technique is that it's fast and conducted online with mass spectrometry detection.I first had the idea for this method when I opened a bottle of carbonated drink on a sunny day. The bubbles of carbon dioxide released the aroma of the drink. I felt we could easily reproduce this process in the laboratory.To begin this procedure, prepare a stock solution of limonene in ethanol by mixing 10 microliters of limonene with 990 microliters of ethanol. To prepare the real sample, first squeeze fresh lime fruit on a kitchen squeezer to obtain lime juice. Next, mix two milliliters of lime juice in 500 microliters of ethanol.Add LC-MS grade water to a final volume of 10 milliliters and shake the volumetric flask thoroughly. Transfer the prepared sample of diluted lime juice to a 20 milliliter screw top head space glass vial with septum cap. Now, prepare a spiked sample by mixing two milliliters of lime juice, 10 microliters of the limonene stock solution, and 490 microliters of ethanol.Add LC-MS grade water to a final volume of 10 milliliters and shake the volumetric flask thoroughly. Connect a carbon dioxide gas cylinder to the gas supply inlet of a fizzy extraction system. Open the valve in the gas regulator.Then set the output pressure to 1.5 bar. Following this, connect the extraction chamber outlet to the ion source inlet. Then connect the fizzy extraction system to a 12 volt power supply.Set up the data acquisition software of a triple quadropole mass spectrometer connected to the fizzy extraction system. Set the desolvation line temperature to 250 degrees Celsius and the flow rate of drying gas to 15 liters per minute. Then select the MS data acquisition method file.Check that the collision voltage is minus 20 volts, the precursor ion master charge ratio is 137, and the fragment ion master charge ratios are 81 and 95. Then click on the Start Single Run button. Place a sample vial in the fizzy extraction system by using the screw mount.Press the start button on the LCD shield of the fizzy extraction system. While the automated fizzy extraction process is proceeding, observe development of ion signals on the screen of the triple quadropole mass spectrometer. Carbon dioxide is pressurized in the simple Then the simple chamber is decompressed which leads to effervescence.After the fizzy extraction process is complete, unscrew the sample vial from the system. Wipe the sample stirring spindle with cellulose tissue. Then wash the spindle with ethanol and wipe it with cellulose tissue.After switching off the power supply, disconnect the fizzy extraction outlet tube from the ion source. Then close the valve of the gas cylinder and disconnect the gas tubing. Export extracted ion currents for the master charge ratio 81 from the triple quadropole mass spectrometer's data acquisition software to ASCII files.First, click on Select Folder and choose the data file. Click on the File tab, select Export Data and select Export Data as ASCII. Select Output File, select the file path, and click on Open.Then select MS Chromatogram(MC)To import the data into the peak integration software and measure the peak areas, select the option Import from the File tab. Open the data file, click on the Yes button, and select the data in the X and Y columns. Then click on OK and select the option Auto Fit Peaks One Residuals.Now, fit the extraction peak semi-automatically making sure that the fitted curve follows the experimental data points. Select the options List Peak Estimates and then ASCII Editor. Copy the fitting results to clipboard.To input the peak areas in data analysis software, first input the peak area values in the Y column and the concentration values in the X column. Under the Plot tab, select Symbol and Scatter. Then select Fitting and Fit Linear from the Analysis tab.The temporal peak areas of extraction events are correlated with concentrations of the analytes in the liquid sample subjected to fizzy extraction which enables quantitative analysis. In this experiment, double standard edition was performed to demonstrate the quantitative capabilities of the technique. A plot relating temporal peaks areas with the concentration of limonene standard added to the diluted lime juice sample is shown here.Based on the obtained slope and intercept values, the concentration of limonene in the diluted lime juice sample was 8.51 times 10 to the minus five moles per liter. After multiplying by the dilution factor, the concentration of limonene in the original lime juice sample was 4.26 times 10 to the minus four moles per liter. Once mastered, this technique can be done in less than 10 minutes if it is performed properly.While attempting this procedure, it's important to remember to set the experimental parameters correctly. After watching this video, you should have a good understanding of how to set up fizzy extraction equipment and perform extractions of real samples. Don't forget that working with compressed gas can be extremely hazardous and precautions such as wearing safety goggles should always be taken while performing this procedure.

Research

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Chemistry

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The high pressure sapphire cell apparatus was constructed to visually determine the composition of multiphase systems without physical sampling. ...

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Analyse av flyktige og oksidasjon Sensitive Forbindelser hjelp av en kald Inlet System og Electron Impact massespektrometri

This video presents a protocol for the mass spectrometrical analysis of volatile and oxidation sensitive compounds using electron impact ionization. The ...

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En studie av kompleks av Mercury (II) med Dicysteinyl tetrapeptidene av elektrosprayionisering massespektrometri

In this study we evaluated a method for the characterization of complexes, formed in different relative ratios of mercury(II) to dicysteinyl tetrapeptide, ...

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This protocol describes the specific techniques used for the characterization of reducing end (RE) and internal region glycosyl sequence(s) of ...

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Visualisering av Ambient massespektrometri med bruk av Schlieren Photography

This manuscript outlines how to visualize mass spectrometry ambient ionization sources using schlieren photography. In order to properly optimize the mass ...

Real-time Breath Analysis by Using Secondary Nanoelectrospray Ionization Coupled to High Resolution Mass Spectrometry

Sanntid pusten analyse ved hjelp av sekundære Nanoelectrospray Ionization koblet til høy oppløsning massespektrometri

Exhaled volatile organic compounds (VOCs) have aroused considerable interest, since they can serve as biomarkers for disease diagnosis and environmental ...

Characterization of Synthetic Polymers via Matrix Assisted Laser Desorption Ionization Time of Flight (MALDI-TOF) Mass Spectrometry

Characterization of Synthetic Polymers via Matrix Assisted Laser Desorption Ionization Time of Flight MALDI-TOF Mass Spectrometry

Karakteristikk av syntetiske polymerer via Matrix assistert Laser desorpsjon Ionization tiden av fly (MALDI-TOF) massespektrometri

There are many techniques that can be employed in the characterization of synthetic homopolymers, but few provide as useful of information for end group ...

An Efficient Sample Preparation Method to Enhance Carbohydrate Ion Signals in Matrix-assisted Laser Desorption/Ionization Mass Spectrometry

En effektiv utvalg forberedelse metode for å forbedre karbohydrater Ion signaler i Matrix-assistert Laser desorpsjon/ionisering massespektrometri

Sample preparation is a critical process in mass spectrometry (MS) analysis of carbohydrates. Although matrix-assisted laser desorption/ionization (MALDI) ...

High-throughput and Comprehensive Drug Surveillance Using Multisegment Injection-Capillary Electrophoresis-Mass Spectrometry

Høy gjennomstrømming og omfattende narkotika overvåkning bruker Multisegment injeksjon-kapillære geleelektroforese massespektrometri

New analytical methods are urgently needed to enable high-throughput, yet comprehensive drug screening, given an alarming opioid and prescription drug ...