Name: chemical analysis of water-accommodated fractions of crude oil spills using tims-ft-icr ms
Uploaded: 2017-03-03T14:00:00
Description: Watch this Scientific Journal Video about Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS at JoVE.com

この作品は、国立衛生研究所（FFLへの助成金番号R00GM106414）によってサポートされていました。私たちは、彼らのサポートのためにフロリダ国際大学の高度な質量分析施設を承認したいと思います。

低エネルギーの水を収容する画分の調製（LEWAF） <ol><li>任意の潜在的な汚染物質を除去するために、塩化メチレンでボトルを洗浄することにより清浄な2リットルのアスピレーターボトル。 </li><li> 、塩化メチレン50mLでボトルを記入し、それらを閉じて、30秒間攪拌します。適切な廃棄物容器にそれらを排出します。合計3回の洗浄のために繰り返します。 </li><li>照射曝露と対照サンプルのよ?...

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プロトコル内の重要なステップ LEWAFsの化学的複雑さは正確に自然に発生するものを反映するために実験室での実験のための順序で正確な準備が必要です。データの有効性評価は、三つの基準にかかっ：（ 例えば、LEWAFの準備、サンプリング、抽出、および分析のための試料調製）を取り扱うサンプル全体のアーティファクトの導入を最小限に抑え、暗いコントロー?...

原油への環境暴露の多数の供給源は、自然の原因からと人為的暴露からの両方があります。環境への放出の際に、特に海で、原油は、表面に油膜の形成、大気中への揮発性成分の損失、及び沈降して、パーティショニングを受けることができます。しかし、古典的可溶化しない難溶性油と水が発生し、そしてこの混合物を低エネルギーの混合は、低エネルギーの水収容フラクション（LEWAF）と呼ばれるものを形成します。水中の油成分の可溶化は、典型的には、太陽放射への油 - 水界面の露光中に増強されます。海の原油の写真可溶化は、太陽放射および/またはによる酵素分解1,2のこの曝露に起因する有意な化学変化を受けることができます。これらの化学的変化を理解し、<html>彼らはバルクマトリックス（ すなわち、原油）の存在下で生じるどのようにこの暴露が環境に影響を緩和するための基本です。 以前の研究では、原油は、酸素、生物に害を与える汚染物質の毒性の高いソースを表し、特に多環式芳香族炭化水素（PAH）を受ける生物蓄積を受け、生物活性3、5、6であることを示しています。彼らは唯一のバルクマトリックスの存在下で生じるので、異なる酸素化プロセスの製品を理解することは困難です。したがって、単一の、標準的な分析は、自然界に起こる変化の代表ではないかもしれません。 LEWAFの製造は、環境設定で起こる自然のプロセスを複製する必要があります。特に興味深いのは、太陽放射による発生のPAHの酸素、です。 トン &quot;&gt;水収納フラクションの研究における第二の課題は、サンプル中の異なる化学成分の分子同定である。その高い質量と酸素の程度によって引き起こされるサンプルの複雑、に、酸素生成物であります例えば、FT-ICR MS（伝統的な分析は、MS分析7,8と組み合わせたガスクロマトグラフィーにより行った。別のアプローチは、超高質量分解能MS技術を利用することによって、試料の化学式の変化を特徴づけるために、典型的には不向き）。FT-ICR MSにTIMSを結合することにより、MSドメイン内のアイソバリック分離に加えて、イオン移動度分光分析（IMS）の寸法は、サンプル9、10、11中に存在する異なる異性体用分離及び特性情報を提供します。大気圧レーザーと組み合わせイオン化（APLI）ソース、分析がPAH類が正確に12、13を特徴とする受けることの変更を可能にする、サンプルで見つかった共役系分子に選択的であり得ます。 この研究では、油成分の変換プロセスを研究するために、光照射をLEWAFsの調製のためのプロトコールを記載します。我々はまた、光照射時に生じる変化、ならびにサンプル抽出のための手順を示します。また、光への曝露の関数としてLEWAF中のPAHを特徴づけるためにFT-ICR MSと相まってTIMSとAPLIの使用を紹介します。

<table border="0" cellpadding="0" cellspacing="0" width="915">
	<tbody>
		<tr height="20">
			<td height="20" style="height:20px;width:228px;">Reagents</td>
			<td style="width:156px;"></td>
			<td style="width:156px;"></td>
			<td style="width:375px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">methylene chloride</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">methanol</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">toluene</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Na2SO4</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Crude oil</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Instant Ocean&#174;</td>
			<td>Aquarium Systems</td>
			<td></td>
			<td>33 ppt salinity with 0.45 &#956;m pore filtration&#160;</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Name&#160;</td>
			<td>Company</td>
			<td>Catalog Number</td>
			<td>Comments</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Equipment</td>
			<td></td>
			<td></td>
			<td></td>
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		<tr height="20">
			<td height="20" style="height:20px;">Suntext XLS+</td>
			<td>Atlas Chicalo Ill, USA</td>
			<td></td>
			<td>1500 w xeon arc lamp, light intensity of 765 W/m2&#160;</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Atmospheric Pressure Laser Ionization</td>
			<td>Bruker Daltonics Inc, MA</td>
			<td></td>
			<td>Note a 266 nm laser is used</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">TIMS-FT-ICR MS Instrument</td>
			<td>Bruker Daltonics Inc, MA</td>
			<td></td>
			<td>The set up we had consisted of a 7T magnet with an infinity cell</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Name&#160;</td>
			<td>Company</td>
			<td>Catalog Number</td>
			<td>Comments</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Software</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">DataAnalysis 4.2</td>
			<td>Bruker Daltonics Inc, MA</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Python 2.7</td>
			<td></td>
			<td></td>
			<td>Requires Numpy, Scipy, Pandas, glob, oct2py, and os</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Octave 4.0</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
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chemical analysis of water-accommodated fractions of crude oil spills using tims-ft-icr ms

複数の化学プロセスはまた、経時的に発生する化学反応を海水中に組み込まれ、どのように原油を制御します。このシステムを研究することは正確に自然界に存在する水を収容画分の自然形成を再現するために、サンプルの慎重な準備が必要です。低エネルギーの水収容フラクション（LEWAF）を慎重に設定された比率で原油と水とを混合することによって調製されます。吸引瓶は、次に照射され、設定された時点で、水を採取し、標準的な技術を用いて抽出しました。第二の課題を考慮に時間をかけて起こる化学的変化を取らなければならないサンプルの代表的な特性評価、です。 LEWAFの芳香族留分の標的分析は、特注のトラップされたイオン移動度分光分析、フーリエ変換イオンサイクロトロン共鳴質量分析計（TIMS-FTに接続された大気圧レーザーイオン化源を用いて行うことができます-ICR MS）。 TIMS-FT-ICR MS分析は、さらに、それらの衝突断面積（CCS）と化学式の異性体成分の同定を可能にする高解像度のイオン移動度と超高分解能MS分析を、提供します。結果は、油 - 水混合物が光に曝されるように、表面油のかなりの光可溶化は、水の中に存在することを示しています。時間が経つにつれて、可溶化された分子の化学変換は、典型的には、基油で観察されたよりも窒素と高い酸素含有量を有​​するものが有利で硫黄含有種の同定の数の減少で、行われます。

m / zとTIMSトラップ電圧に基づいて、2次元スペクトルにおけるTIMS-FT-ICR MSの結果によってLEWAF分析。化学式の分布とIMS（ 図1参照）によって同定異性寄与によって観察されるように種々の時点で採取した試料の各々は、従って、変化の化学組成に基づいて特徴付けることができます。典型的には、 のm / zの情報を分析し、ピークに基本式を割り...

Watch this Scientific Journal Video about Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS at JoVE.com

Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS

時間をかけて、この複雑な混合物は、化学変換を受けるので、原油の低エネルギーの水収容フラクション（LEWAF）は、分析する困難なシステムです。このプロトコルはLEWAFサンプルの調製のために捕捉されたイオン移動度分光分析、FT-ICR MSにより光照射および化学分析を行うための方法を示す図です。

原油の水を収容する画分の化学分析は、TIMS-FT-ICR MSを用いて流出します

Multiple chemical processes control how crude oil is incorporated into seawater and also the chemical reactions that occur overtime. Studying this system ...

The overall goal of these experiments is to illustrate the analytical advantages of enabling emerging technologies based on TIMS-FT-ICR MS for the molecular characterization of complex mixtures, such as water-accommodated fractions for crude oils. The TIMS-FT-ICR MS coupling combines two of the most comprehensive orthogonal and alluvial techniques for the analysis of complex mixtures. TIMS-FT-ICR MS coupling permits in a single analysis the characterization of thousands of molecular components with mobility resolving powers of over 150, mass resolution of 500, 000, and sub-ppm mass accuracy.TIMS-FT-ICR MS enables the separation, identification, and quantitation at the molecular level of complex mixtures, based on differences in size, charge and mass with minimal sample appropriation. To begin the LEGAF preparation, add 50 milliliters of dicholomethane to a two liter glass aspirator bottle. Close the bottle and agitate the bottle for 30 seconds.Discard the dichloromethane wash, and repeat this process two more times. Wash one more two liter aspirator bottle in this way, then add about 1.6 liters of filtered artificial seawater with a salinity of 33 parts per thousand to each bottle. Add a stir bar, and then use a gas-tight syringe to add sufficient crude oil sample to each bottle to achieve a final concentration of one gram per liter of oil and seawater.Wrap the bottles in aluminum foil to exclude light, and stir the mixtures at approximately 100 RPM for 24 hours to finish preparing the LEWAF. It's important that care is used when first mixing the oil and water to avoid over-mixing the solution. Next, unwrap one of the LEWAF bottles in aluminum foil, leaving one as the dark control.Place the bottles in the solar irradiator with the temperature set to maintain the samples at 25 degrees Celsius. Irradiate the mixtures continuously for the desired experiment length. At set intervals during the experiment, obtain 150 milliliter fractions from each bottle by uncorking the bottle and opening the drain valve.Extract each sample aliquot using 50 milliliters of dichloromethane three times using a separatory funnel. Shake the funnel for two minutes each time, remembering to regularly vent the funnel to avoid pressure buildup. Drain the sample into a flat-bottom flask through a funnel containing sulfate and rinse the sodium sulfate with additional DCM.Concentrate the extract to 15 milliliters using a hot water bath set at 58 degrees Celsius. Transfer the concentrate into a concentration tube, rinsing the flask with DCM. Concentrate each sample to one milliliter under a gentle stream of nitrogen gas.For each concentrated sample, using a glass positive displacement micropipette, add 990 microliters of a one to one by volume mixture of methanol and toluene to a glass vial. Then mix in 10 microliters of the sample. To begin the FTR-ICR MS analysis, set the instrument to Operate mode.Draw a sample into a sample syringe. Set the infusion rate to 200 microliters per hour, the nebulizer pressure to two bar, and the vaporizer temperature to 300 degrees Celsius. Set the dry gas rate to 1.2 liters per minute and the temperature to 220 degrees Celsius.Then set the instrument to Tune mode. Based on the resulting spectrum adjust the instrument parameters and recalibrate the mass spectrometer to improve the ion transmission and detection for the desired range of mass to charge ratios. Once the instrument parameters have been optimized, exit Tune mode.Set the desired number of scans to be average per mass spectrum, and then acquire the spectrum. To begin the trapped ion mobility spectrometry analysis turn on the external breaker to the TIMS instrument to engage TIMS mode. Set the FT-ICR instrument to chromatography mode.Turn on the supplementary roughing pump and set the inlet and outlet pressures to the desired values using the TIMS control valve. Allow the pump to warm up for at least three hours, then perform a fast sweep over a wide voltage range at a low IMS and MS resolution to identify the needed voltage range for the analysis. Once the range has been identified, set the voltage per frame to 0.1 volts.Set the number of frames to cover the entirety of the DeltaV ramp and run the analysis. After performing the analyses, process the data with the appropriate software and scripts to determine the chemical composition and mobility values of identified peaks. After sunlight irradiation of an LEWAF of a crude oil sample, changes in the chemical complexity are observed as a function of exposure time.This complexity was detected and visualized in a 2D spectrum based on mass to charge ratio and ion mobility. The use of APLI resulted in greater analytical sensitivity to molecules with double bonds. Four molecular classes were identified in the sample.Distribution plots of double bond equivalents as a function of the number of carbons were used to monitor changes in the molecular composition over time. Two-dimensional plots of inverse mobility versus carbon number were created, with the double bond equivalents represented as the color of each point. Linear trends were observed for each of the four common molecular classes.After watching this video you should have a good understanding of the basic steps and unique advantages of APLI-TIMS-FT-ICR MS for the analysis of LEWAF samples as well as other complex mixtures. While attempting this procedure it's important to remember that sample integrity, such as reducing sources of contamination, is fundamental for accurate results. The characterization at the molecular level of the water-accommodated fractions of crude oils, the transformation products, and their fate during exposure to sunlight in the ocean is of the utmost environmental importance.Compared to other separation techniques such as liquid chromatography and gas chromatography, TIMS separation occurs in a shorter time scale, and is timing dependent, which permits better coupling with ultra high resolution MS analyzers while providing collision cross sections and chemical formulas in a single analysis. The generation of new comprehensive analytical tools for the analysis of complex mixtures at molecular level, such as TIMS-FT-ICR MS has great implications for our understanding of the chemical transformations and fate of crude oil in the ocean.

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SCIENTISTS IN ACTION

Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

Hの測定<sub&gt; 2</sub&gt;原油や多次元ガスクロマトグラフィーを用いて原油ヘッドスペース中のSは、学部長は、スイッチングおよび硫黄選択的検出

A method for the analysis of dissolved hydrogen sulfide in crude oil samples is demonstrated using gas chromatography. In order to effectively eliminate ...

環境学

LC-MS Analysis of Human Platelets as a Platform for Studying Mitochondrial Metabolism

ミトコンドリア代謝を研究するためのプラットフォームとしてのヒト血小板のLC-MS分析

Perturbed mitochondrial metabolism has received renewed interest as playing a causative role in a range of diseases. Probing alterations to metabolic ...

Methods of Soil Resampling to Monitor Changes in the Chemical Concentrations of Forest Soils

森林土壌の化学濃度の変化を監視するための土壌リサンプリングの方法

Recent soils research has shown that important chemical soil characteristics can change in less than a decade, often the result of broad environmental ...

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

Measurement of the Rheology of Crude Oil in Equilibrium with CO2 at Reservoir Conditions

COとの平衡状態における原油のレオロジーの測定<sub&gt; 2</sub&gt;貯水池の条件で

A rheometer system to measure the rheology of crude oil in equilibrium with carbon dioxide (CO2) at high temperatures and pressures is described. The ...

Dispersion of Nanomaterials in Aqueous Media: Towards Protocol Optimization

水溶液中におけるナノ材料の分散: プロトコルの最適化に向けて

The sonication process is commonly used for de-agglomerating and dispersing nanomaterials in aqueous based media, necessary to improve homogeneity and ...

Microfluidic Devices for Characterizing Pore-scale Event Processes in Porous Media for Oil Recovery Applications

油回収用多孔質媒体における細孔スケール イベント プロセスを特徴づけるためのマイクロ流体デバイス

Microfluidic devices are versatile tools for studying transport processes at a microscopic scale. A demand exists for microfluidic devices that are ...

The Effect of the Application of Thyme Essential Oil on Microbial Load During Meat Drying

タイムのエッセンシャル オイルのアプリケーションの肉乾燥中の微生物負荷に及ぼす影響

Meat is a high protein meal that is used in the preparation of jerky, a popular food snack, where preservation and safety are important. To assure food ...

Identification of Pharmaceuticals in The Aquatic Environment Using HPLC-ESI-Q-TOF-MS and Elimination of Erythromycin Through Photo-Induced Degradation

高速液体クロマトグラフィー ESI Q TOF MS と光誘起分解によるエリスロマイシンの除去を使用して水生環境における医薬品の識別

Monitoring pharmaceuticals throughout the water cycle is becoming increasingly important for the aquatic environment and eventually for human health. ...

A Novel Method for the Pentosan Analysis Present in Jute Biomass and Its Conversion into Sugar Monomers Using Acidic Ionic Liquid

ペントサン解析手法ジュート バイオマスと酸性イオン液体を用いた糖モノマーへの変換に存在

Recently, ionic liquids (ILs) are used for biomass valorization into valuable chemicals because of their remarkable properties such as thermal stability, ...

Isolation of Mandibular Gland Reservoir Contents from Bornean 'Exploding Ants' (Formicidae) for Volatilome Analysis by GC-MS and MetaboliteDetector

Isolation of Mandibular Gland Reservoir Contents from Bornean 'Exploding Ants' Formicidae for Volatilome Analysis by GC-MS and MetaboliteDetector

ボルネオから下顎腺貯留層内容の分離 ' GC MS と MetaboliteDetector による Volatilome 解析のためアリの (守) を爆発

The aim of this manuscript is to present a protocol describing the metabolomic analysis of Bornean &#39;exploding ants&#39; belonging to the Colobopsis ...