로버트 버거 (Philipps 대학 Marburg, 독일)를 감사 우리가 우리의 데이터와 분자 카이랄성의 해석에 대 한 논의 일반적 영감. 우리는 제공 하는 샘플에 대 한 ZHAW Wädenswil (스위스)에서 줄리아 Kiedrowski 알렉산더 Schießer와 마이클 Reggelin TU 다름슈타트 (독일)에서 뿐 아니라 벤자민 Spenger, 마누엘 Mazenauer, Jürgen Stohner 감사.
프로젝트 초점 ELCH (랄 시스템의 전자 역학)와 연방 교육부의 연구 (BMBF) 아래 과학 · 경제 우수 헤센 주 이니셔티브에 의해 지원 되었다. MS는 아돌프 메 재단이 재정 지원을 인정 한다.

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Phys. 13, 7024-7036 (2010).</li><li>Ablikim, U., 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=Identification+of+absolute+geometries+of+cis+and+trans+molecular+isomers+by+Coulomb+Explosion+Imaging.">Identification of absolute geometries of cis and trans molecular isomers by Coulomb Explosion Imaging.</a> Sci. Rep. 6, 38202 (2016).</li></ol>

저자 아무 경쟁 관심사를 선언합니다.

때문에 다양 한 구성 요소, COLTRIMS 설치 필요 전문 기술, 진공 기술, 입자 감지, 빠른 전자 및 데이터 분석의 분야에서 특히의 다소 높은 수준을 합니다. 하기 전에 복잡 한 종족의 수사에, 그것은 따라서 수 철저 하 게 확인 한다 설치 예: 수행 하 고 2 원자 또는 triatomic 종에 측정 분석 하 여 제대로 실행 되는 경우.
레이저 펄스와 분자 제트 오버랩의 기간과 강도 최적화 ?...

카이랄성은 150 년 이상에 대 한 매혹적인 연구 된 우리의 본성의 기능입니다. 19토 륨 세기, 파스퇴르, van't Hoff 등 분자 슈퍼-imposable-우리의 왼쪽 손과 오른쪽 처럼 되지 않은 두 개의 미러 이미지 구조에서 발생할 수 있습니다 발견. 이 속성 '랄', '손'에 대 한 그리스어 단어에서 불리 했다.
지금까지, 열역학 속성 또는 왼쪽 및 오른 형태 (는 두 ' 상체')의 에너지 레벨 차이가 발견 되었습니다. 주어진된 샘플의 handedness를 분석 하 고는 상체 분리, 다른 카이 랄 분자와 상호 작용 사용할 수 있습니다, 예를 들어 다양 한 chromatographical 방식에서 이루어집니다. 1 (진동) 원형이 색 성, (V) CD 등 광 회전 분산, 오드, Chiroptical 방법 정기적으로 상체를 구분 하기 위해 고용 됩니다. 2
그것은 미세한 구조의 결정에 관해서 라면, 이러한 기술 예: 양자 화학 계산에서에서 추가 정보가 필요. 직접 절대 구성 결정에 널리 허용 되는 유일한 기술이 이다 변칙 엑스레이 회절. 3
그것은 최근에 보였다 간단한 카이 랄의 절대적인 구성 쿨롱 폭발 영상에 의해 결정 될 수 있다. 4 , 5 이 방법에서는, 기체에서 분자는 곱하면 이온 수 있도록 나머지 코어는 강력 하 게 서로 격퇴. 이 반발 분자의 빠른 조각화 ('폭발') 이끌어 낸다. 방향과 크기-작은 분자에 대 한 분자의 구조를 조각 결합체 상관의 운동량 방향 일치 의외로 잘 본드 축. 분자 구조 결정에 대 한 쿨롱 폭발은 분자 이온 빔 가속기에서를 사용 하 여 개척 되었습니다. 6 이 빔 포 일 기술은 최근에 랄 인식에 대 한 적용. 7
변칙 엑스레이 회절, 반대로 샘플 결정 하지만 가스 단계에서 제공 되지 않아야 합니다. 이것은 쿨롱 폭발 접근 휘발성 종족에 대 한 적합 하 고 따라서 x 선 회절을 보완 합니다. 경우에 따라 handedness도 개별 분자에 대 한 확인할 수 있습니다.
실제로, 분자 구조의 정확한 재건 메탄 파생 상품, 예를 들면 중앙 탄소와 다른 치환 기 분자에도 어려운 입증 했다. 이것은 사실 조각 사이 상호 작용은 정확히 Coulombic 모든 채권 동시에 휴식에 기인 합니다. 특히 상체, 사이 구별을 stereochemical 정보를 얻기 위하여이 재건 다행히 필요는 없습니다. 대신, 다른 파편의 기세 벡터 수익률은 왼쪽 및 오른 분자에 대 한 수량 상관 될 수 있다. 신뢰할 수 있는 결과를 얻으려면, 적어도 4 개의 단편 결합체를 기록 해야 합니다.
이 기세 정보를 측정 하기 위해서는 한-그리고 한-분자 휴식-최대에서 파편 단일 측정 단계에서 검색 될 수 있다. 이 상태는 일반적으로 '일치 검색' 이라고 합니다. 또한, 방출 방향 있다 분석할 시간과 조각의 위치를 기록 하는 것에 금액 리스트 모드 데이터 형식에 영향을.
원자와 분자 물리학, 기술 개발 되었다 대량 분리 및 시간 및 위치에 민감한 멀티 히트 탐지기 정전기 분석기를 사용 하 여 측정의이 접근을 구현 하는. 가장 눈에 띄는 COLTRIMS (찬 대상 반동 이온 추진력 분광학) 설치-라고 반응 현미경입니다. 8 , 9 실험의이 종류에 대 한 스케치는 그림 1에서 주어진 다. 뿐만 아니라 전자를 기록할 수 있는 표준 COLTRIMS, 반대로 쿨롱 폭발 이미징 이온 검출기를을 요구 한다.
분석기와 검출기 초고 진공에서 마운트 (&#60; 1 x 10-9 hPa) 잔류 가스에서 이온의 생성을 피하기 위해. 샘플의 단일 분자 만든 초음속 팽창에 의해 가스 무료 분자 jet를 통해 제공 됩니다: 증기압, 덕 분자 진공으로 소형 노즐 (약 50 µ m 직경) 통해 확장. 실험, 소스 챔버의이 부분은 일반적으로 두 개의 스키와 차동 펌핑된 단계 상호 작용 영역에서 분리 된다. 추가 섹션을 펌핑 차동은 가스 제트기를 덤프 하 고 따라서 상호 작용 영역에 배경 가스를 피하기 위해 상호 작용 지역 뒤에 위치 해 있습니다.
이온화 방사선 분자 제트 미만 90 °로 교차합니다. 싱크 로트 론 방사선, 빠른 이온 또는 전자 충격 가능한 '발사체' 쿨롱 폭발을 유도 하는 있지만 대부분 실험실 요즘 펨 레이저 펄스를 사용 합니다.
다음 프로토콜은 이온과 펨 레이저의 일치 이미징에 대 한 실행 설치 실험실에서 사용할 수 있는 가정 합니다. 4 개 또는 5 개의 조각으로 쿨롱 폭발을 유도 하는 데 필요한 최대 강도 6 x 1014 W/c m2의 순서 여야 합니다. 상당히 긴 측정을 방지 하려면 레이저의 반복 속도 10khz 이상 이어야 한다. 이것이 중요 한 한편으로, 일치 탐지 수만 수 ascertained 레이저 초점의 조각화에 대 한 확률은 크게 레이저 펄스 (이상적으로 하지 10% 이상) 당 1 아래 경우 때문에. 총 조각화 비율, 다른 한편으로, 해서는 안됩니다 몇 kHz 보다 낮은 있기 때문에 관련 multifragmentation 통로의 공유는 일반적으로 10-4. 으로 장려 사실 원리 이미 단일 조각 이벤트는 enantiopure 샘플의 구성을 식별 하기에 충분 및 몇 백의 그 검출에 상체의 풍부를 결정 하기 위해 수 있습니다 언급 해야 한 알 수 없는 enantiomeric 구성의 샘플입니다.

<table border="0" cellpadding="0" cellspacing="0" width="599">
	<tbody>
		<tr height="31">
			<td height="31" style="height:31px;width:179px;">CHBrCl2</td>
			<td style="width:93px;">SigmaAldrich</td>
			<td style="width:147px;">139181-10G</td>
			<td style="width:180px;">or other suitable sample</td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:179px;">femtosecond laser system</td>
			<td>KMLabs</td>
			<td style="width:147px;">Wyvern500</td>
			<td style="width:180px;"></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:179px;">High-reflective mirrors</td>
			<td>EKSMA</td>
			<td style="width:147px;">042-0800</td>
			<td style="width:180px;"></td>
		</tr>
		<tr height="31">
			<td height="31" style="height:31px;width:179px;">mirror mounts</td>
			<td>Newport</td>
			<td style="width:147px;">U100-A-LH-2K&#160;&#160;</td>
			<td style="width:180px;"></td>
		</tr>
		<tr height="35">
			<td height="35" style="height:35px;width:179px;">focusing mirror (protected silver, f = 75 mm)</td>
			<td>Thorlabs&#160;</td>
			<td style="width:147px;">CM254-075-P01</td>
			<td style="width:180px;">(if available: f = 60 mm)</td>
		</tr>
		<tr height="51">
			<td height="51" style="height:51px;width:179px;">COLTRIMS spectrometer, including electronics and data acquisition system</td>
			<td>RoentDek</td>
			<td style="width:147px;">custom</td>
			<td style="width:180px;">contrary to the standard COLTRIMS, only one detector is needed</td>
		</tr>
	</tbody>
</table>

coulomb explosion imaging as a tool to distinguish between stereoisomers

이 기사에서는 COLTRIMS (찬 대상 반동 이온 추진력 분광학) 또는 "반응 현미경" 기술을 사용 하는 방법을 개별 분자의 수준에서 간단한 카이 랄의 상체 (stereoisomers) 사이 구별 하. 이 방법에서는, 샘플의 기체 분자 제트 진공 챔버로 확장 하 고 펨 (fs) 레이저 펄스와 교차. 펄스의 강도 높은 여러 이온화, 여러 양이온 (긍정적으로 위탁된) 파편을 생성 하는 소위 쿨롱 폭발 점화를 빨리 이끌어 낸다. 정전기 필드 가이드 시간 및 위치에 민감한 검출기에 이러한 양이온. 시간의 비행 질량 분석기와 마찬가지로, 각 이온의 도착 시간 그것의 질량에 대 한 정보를 생성합니다. 흑자로 정전기 필드는 방출 방향과 조각화 후 운동 에너지 이어질 유사 비행 시간 및 영향 위치 검출기에 방식으로 조정 됩니다.
각 이온 충격 감지기;에 전자 신호를 생성 이 신호는 높은 주파수 전자 처리 하 고는 컴퓨터에서 이벤트에 의해 이벤트를 기록. 등록 된 데이터는 영향 시간과 위치에 해당합니다. 이러한 데이터는 에너지와 각 조각의 방출 방향을 계산할 수 있습니다. 이러한 값은 조사, 즉 채권 길이 결정 분자에 의해 분자 다른 이성질체 기능과 간단한 카이 랄 종의 handedness를 수 있도록 원자의 상대적 위치를 분자의 구조적 속성 관련이 있습니다.

이 부분에서 우리는 halomethanes에 대 한 결과 보여줍니다. 이러한 종의 원리 증명 실험 그들의 단순 하 고 높은 증기 압력 때문에 이상적입니다. 한편, 더 복잡 한 종 halothane 여러 이온화를 유도 하는 싱크 로트 론 소스에서 단일 소프트-x-선 광자를 사용 하 여 조사 했다. 14
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Watch this Scientific Journal Video about Coulomb Explosion Imaging as a Tool to Distinguish Between Stereoisomers at JoVE.com

Coulomb Explosion Imaging as a Tool to Distinguish Between Stereoisomers

Stereoisomers 사이 구별 하는 도구로 쿨롱 폭발 영상

작은 키 랄 종에 대 한 쿨롱 폭발 이미징 개별 분자의 handedness를 결정 하는 새로운 접근을 제공 합니다.

This article shows how the COLTRIMS (Cold Target Recoil Ion Momentum Spectroscopy) or the "reaction microscope" technique can be used to distinguish ...

coulomb-explosion-imaging-as-tool-to-distinguish-between

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Organic Chemistry

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Unit 1

Transition Metals and Coordination Complexes

Stereoisomerism

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9.0K 조회수.  Goethe-Universität Frankfurt am Main. 작은 키 랄 종에 대 한 쿨롱 폭발 이미징 개별 분자의 handedness를 결정 하는 새로운 접근을 제공 합니다.

비디오: Coulomb Explosion Imaging as a Tool to Distinguish Between Stereoisomers

Rapid Colorimetric Assays to Qualitatively Distinguish RNA and DNA in Biomolecular Samples

Biochemical experimentation generally requires accurate knowledge, at an early stage, of the nucleic acid, protein, and other biomolecular components in potentially heterogeneous specimens. Nucleic acids can be detected via several established approaches, including analytical methods that are spectrophotometric (e.g., A260), fluorometric (e.g., binding of fluorescent dyes), or colorimetric (nucleoside-specific chromogenic chemical reactions).1 Though it cannot readily distinguish RNA from DNA, the A260/A280 ratio is commonly employed, as it offers a simple and rapid2 assessment of the relative content of nucleic acid, which absorbs predominantly near 260 nm and protein, which absorbs primarily near 280 nm. Ratios &lt; 0.8 are taken as indicative of 'pure' protein specimens, while pure nucleic acid (NA) is characterized by ratios &gt; 1.53.
However, there are scenarios in which the protein/NA content cannot be as clearly or reliably inferred from simple uv-vis spectrophotometric measurements. For instance, (i) samples may contain one or more proteins which are relatively devoid of the aromatic amino acids responsible for absorption at &asymp;280 nm (Trp, Tyr, Phe), as is the case with some small RNA-binding proteins, and (ii) samples can exhibit intermediate A260/A280 ratios (~0.8 &lt; ~1.5), where the protein/NA content is far less clear and may even reflect some high-affinity association between the protein and NA components. For such scenarios, we describe herein a suite of colorimetric assays to rapidly distinguish RNA, DNA, and reducing sugars in a potentially mixed sample of biomolecules. The methods rely on the differential sensitivity of pentoses and other carbohydrates to Benedict's, Bial's (orcinol), and Dische's (diphenylamine) reagents; the streamlined protocols can be completed in a matter of minutes, without any additional steps of having to isolate the components. The assays can be performed in parallel to differentiate between RNA and DNA, as well as indicate the presence of free reducing sugars such as glucose, fructose, and ribose (Figure 1).

A suite of colorimetric assays is described for rapidly distinguishing protein, RNA, DNA, and reducing sugars in potentially heterogeneous biomolecular samples.

신속한 Colorimetric Assays는 질적 Biomolecular 샘플에서 RNA와 DNA를 구별 할

Biochemical experimentation generally requires accurate knowledge, at an early stage, of the nucleic acid, protein, and other biomolecular components in ...

연구

화학

Real-time Monitoring of Reactions Performed Using Continuous-flow Processing: The Preparation of 3-Acetylcoumarin as an Example

By using inline monitoring, it is possible to optimize reactions performed using continuous-flow processing in a simple and rapid way. It is also possible to ensure consistent product quality over time using this technique. We here show how to interface a commercially available flow unit with a Raman spectrometer. The Raman flow cell is placed after the back-pressure regulator, meaning that it can be operated at atmospheric pressure. In addition, the fact that the product stream passes through a length of tubing before entering the flow cell means that the material is at RT. It is important that the spectra are acquired under isothermal conditions since Raman signal intensity is temperature dependent. Having assembled the apparatus, we then show how to monitor a chemical reaction, the piperidine-catalyzed synthesis of 3-acetylcoumarin from salicylaldehyde and ethyl acetoacetate being used as an example. The reaction can be performed over a range of flow rates and temperatures, the in-situ monitoring tool being used to optimize conditions simply and easily.

Real-time monitoring allows for fast optimization of reactions performed using continuous-flow processing. Here the preparation of 3-acetylcoumarin is used as an example. The apparatus for performing in-situ Raman monitoring is described, as are the steps required to optimize the reaction.

연속 흐름 처리를 사용하여 수행 반응의 실시간 모니터링 : 예를 들어 3 Acetylcoumarin의 제조

By using inline monitoring, it is possible to optimize reactions performed using continuous-flow processing in a simple and rapid way. It is also possible ...

Deacetylation Assays to Unravel the Interplay between Sirtuins (SIRT2) and Specific Protein-substrates

Acetylation has emerged as an important post-translational modification (PTM) regulating a plethora of cellular processes and functions. This is further supported by recent findings in high-resolution mass spectrometry based proteomics showing that many new proteins and sites within these proteins can be acetylated. However the identity of the enzymes regulating these proteins and sites is often unknown. Among these enzymes, sirtuins, which belong to the class III histone lysine deacetylases, have attracted great interest as enzymes regulating the acetylome under different physiological or pathophysiological conditions. Here we describe methods to link SIRT2, the cytoplasmic sirtuin, with its substrates including both in vitro and in vivo deacetylation assays. These assays can be applied in studies focused on other members of the sirtuin family to unravel the specific role of sirtuins and are necessary in order to establish the regulatory interplay of specific deacetylases with their substrates as a first step to better understand the role of protein acetylation. Furthermore, such assays can be used to distinguish functional acetylation sites on a protein from what may be non-regulatory acetylated lysines, as well as to examine the interplay between a deacetylase and its substrate in a physiological context.

Deacetylation Assays to Unravel the Interplay between Sirtuins SIRT2 and Specific Protein-substrates

This protocol describes the required steps to execute in vitro and in vivo deacetylation assays in order to establish the role of proteins as specific deacetylation substrates for sirtuins and further study the role of reversible - lysine acetylation as a post-translational modification.

탈 아세틸 화 분석법은 시르 투 인 사이의 상호 작용 (SIRT2) 및 특정 단백질 기판을 해명

Acetylation has emerged as an important post-translational modification (PTM) regulating a plethora of cellular processes and functions. This is further ...

Spin Saturation Transfer Difference NMR (SSTD NMR): A New Tool to Obtain Kinetic Parameters of Chemical Exchange Processes

This detailed protocol describes the new Spin Saturation Transfer Difference Nuclear Magnetic Resonance protocol (SSTD NMR), recently developed in our group to study processes of mutual-site chemical exchange that are difficult to analyze by traditional methods. As the name suggests, this method combines the Spin Saturation Transfer method used for small molecules, with the Saturation Transfer Difference (STD) NMR method employed for the study of protein-ligand interactions, by measuring transient spin saturation transfer along increasing saturation times (build-up curves) in small organic and organometallic molecules undergoing chemical exchange.
Advantages of this method over existing ones are: there is no need to reach coalescence of the exchanging signals; the method can be applied as long as one signal of the exchanging sites is isolated; there is no need to measure T1 or reach steady state saturation; rate constant values are measured directly, and T1 values are obtained in the same experiment, using only one set of experiments.
To test the method, we have studied the dynamics of the hindered rotation of N,N-dimethylamides, for which much data is available for comparison. The thermodynamic parameters obtained using SSTD are very similar to the reported ones (spin-saturation transfer techniques and line-shape analysis). The method can be applied to more challenging substrates that cannot be studied by previous methods.
We envisage that the simple experimental set up and the wide applicability of the method to a great variety of substrates will make this a common technique amongst organic and organometallic chemists without extensive expertise in NMR.

Spin Saturation Transfer Difference NMR SSTD NMR: A New Tool to Obtain Kinetic Parameters of Chemical Exchange Processes

A detailed protocol describing the SSTD NMR method is presented here to help new users apply this new method to obtain the kinetic parameters of their own systems undergoing chemical exchange.

This detailed protocol describes the new Spin Saturation Transfer Difference Nuclear Magnetic Resonance protocol (SSTD NMR), recently developed in our ...

NMR Spectroscopy as a Robust Tool for the Rapid Evaluation of the Lipid Profile of Fish Oil Supplements

The western diet is poor in n-3 fatty acids, therefore the consumption of fish oil supplements is recommended to increase the intake of these essential nutrients. The objective of this work is to demonstrate the qualitative and quantitative analysis of encapsulated fish oil supplements using high-resolution 1H and 13C NMR spectroscopy utilizing two different NMR instruments; a 500 MHz and an 850 MHz instrument. Both proton (1H) and carbon (13C) NMR spectra can be used for the quantitative determination of the major constituents of fish oil supplements. Quantification of the lipids in fish oil supplements is achieved through integration of the appropriate NMR signals in the relevant 1D spectra. Results obtained by 1H and 13C NMR are in good agreement with each other, despite the difference in resolution and sensitivity between the two nuclei and the two instruments. 1H NMR offers a more rapid analysis compared to 13C NMR, as the spectrum can be recorded in less than 1 min, in contrast to 13C NMR analysis, which lasts from 10 min to one hour. The 13C NMR spectrum, however, is much more informative. It can provide quantitative data for a greater number of individual fatty acids and can be used for determining the positional distribution of fatty acids on the glycerol backbone. Both nuclei can provide quantitative information in just one experiment without the need of purification or separation steps. The strength of the magnetic field mostly affects the 1H NMR spectra due to its lower resolution with respect to 13C NMR, however, even lower cost NMR instruments can be efficiently applied as a standard method by the food industry and quality control laboratories.

Here, high-resolution 1H and 13C Nuclear Magnetic Resonance (NMR) spectroscopy was used as a rapid and reliable tool for quantitative and qualitative analysis of encapsulated fish oil supplements.

생선 기름 보충제의 지질 프로필의 신속한 평가를위한 강력한 도구로 NMR 분광학

The western diet is poor in n-3 fatty acids, therefore the consumption of fish oil supplements is recommended to increase the intake of these essential ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

전기 화학 임피던스 분 광 전기 화학 속도 상수 추정을 위한 도구로

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Color Spot Test As a Presumptive Tool for the Rapid Detection of Synthetic Cathinones

Synthetic cathinones are a large class of new psychoactive substances (NPS) that are increasingly prevalent in drug seizures made by law enforcement and other border protection agencies globally. Color testing is a presumptive identification technique indicating the presence or absence of a particular drug class using rapid and uncomplicated chemical methods. Owing to their relatively recent emergence, a color test for the specific identification of synthetic cathinones is not currently available. In this study, we introduce a protocol for the presumptive identification of synthetic cathinones, employing three aqueous reagent solutions: copper(II) nitrate, 2,9-dimethyl-1,10-phenanthroline (neocuproine) and sodium acetate. Small pin-head sized amounts (approximately 0.1-0.2 mg) of the suspected drugs are added to the wells of a porcelain spot plate, and each reagent is then added dropwise sequentially before heating on a hotplate. A color change from very light blue to yellow-orange after 10 min indicates the likely presence of synthetic cathinones. The highly stable and specific test reagent has the potential for use in the presumptive screening of unknown samples for synthetic cathinones in a forensic laboratory. However, the nuisance of an added heating step for the color change result limits the test to laboratory application and decreases the likelihood of an easy translation to field testing.

Here we present a simple, inexpensive, and selective chemical spot test protocol for the detection of synthetic cathinones, a class of new psychoactive substances. The protocol is suitable for use in various areas of law enforcement that encounter illicit material.

색상 합성 Cathinones의 급속 한 탐지에 대 한 추정 도구로 자리 테스트

Synthetic cathinones are a large class of new psychoactive substances (NPS) that are increasingly prevalent in drug seizures made by law enforcement and ...

Automation of a Positron-emission Tomography (PET) Radiotracer Synthesis Protocol for Clinical Production

The development of new positron-emission tomography (PET) tracers is enabling researchers and clinicians to image an increasingly wide array of biological targets and processes. However, the increasing number of different tracers creates challenges for their production at radiopharmacies. While historically it has been practical to dedicate a custom-configured radiosynthesizer and hot cell for the repeated production of each individual tracer, it is becoming necessary to change this workflow. Recent commercial radiosynthesizers based on disposable cassettes/kits for each tracer simplify the production of multiple tracers with one set of equipment by eliminating the need for custom tracer-specific modifications. Furthermore, some of these radiosynthesizers enable the operator to develop and optimize their own synthesis protocols in addition to purchasing commercially-available kits. In this protocol, we describe the general procedure for how the manual synthesis of a new PET tracer can be automated on one of these radiosynthesizers and validated for the production of clinical-grade tracers. As an example, we use the ELIXYS radiosynthesizer, a flexible cassette-based radiochemistry tool that can support both PET tracer development efforts, as well as routine clinical probe manufacturing on the same system, to produce [18F]Clofarabine ([18F]CFA), a PET tracer to measure in vivo deoxycytidine kinase (dCK) enzyme activity. Translating a manual synthesis involves breaking down the synthetic protocol into basic radiochemistry processes that are then translated into intuitive chemistry &#34;unit operations&#34; supported by the synthesizer software. These operations can then rapidly be converted into an automated synthesis program by assembling them using the drag-and-drop interface. After basic testing, the synthesis and purification procedure may require optimization to achieve the desired yield and purity. Once the desired performance is achieved, a validation of the synthesis is carried out to determine its suitability for the production of the radiotracer for clinical use.

Automation of a Positron-emission Tomography PET Radiotracer Synthesis Protocol for Clinical Production

Positron-emission tomography (PET) imaging sites that are involved in multiple early clinical research trials need robust and versatile radiotracer manufacturing capabilities. Using the radiotracer [18F]Clofarabine as an example, we illustrate how to automate the synthesis of a radiotracer using a flexible, cassette-based radiosynthesizer and validate the synthesis for clinical use.

양전자 방출 단층 촬영 (PET) Radiotracer 합성 프로토콜의 임상 생산을 위한 자동화

The development of new positron-emission tomography (PET) tracers is enabling researchers and clinicians to image an increasingly wide array of biological ...

Solid Phase 11C-Methylation, Purification and Formulation for the Production of PET Tracers

Routine production of radiotracers used in positron emission tomography (PET) mostly relies on wet chemistry where the radioactive synthon reacts with a non-radioactive precursor in solution. This approach necessitates purification of the tracer by high performance liquid chromatography (HPLC) followed by reformulation in a biocompatible solvent for human administration. We recently developed a novel 11C-methylation approach for the highly efficient synthesis of carbon-11 labeled PET radiopharmaceuticals, taking advantage of solid phase cartridges as disposable &#34;3-in-1&#34; units for the synthesis, purification and reformulation of the tracers. This approach obviates the use of preparative HPLC and reduces the losses of the tracer in transfer lines and due to radioactive decay. Furthermore, the cartridge-based technique improves synthesis reliability, simplifies the automation process and facilitates compliance with the Good Manufacturing Practice (GMP) requirements. Here, we demonstrate this technique on the example of production of a PET tracer Pittsburgh compound B ([11C]PiB), a gold standard in vivo imaging agent for amyloid plaques in the human brains.

Solid Phase 11C-Methylation, Purification and Formulation for the Production of PET Tracers

We report an efficient carbon-11 radiolabeling technique to produce clinically relevant tracers for Positron Emission Tomography (PET) using solid phase extraction cartridges. 11C-methylating agent is passed through a cartridge preloaded with precursor and successive elution with aqueous ethanol provides chemically and radiochemically pure PET tracers in high radiochemical yields.

PET 트레이서 생산을 위한 고체 상 11C-메틸화, 정제 및 제형

Routine production of radiotracers used in positron emission tomography (PET) mostly relies on wet chemistry where the radioactive synthon reacts with a ...

In situ FTIR Spectroscopy as a Tool for Investigation of Gas/Solid Interaction: Water-Enhanced CO2 Adsorption in UiO-66 Metal-Organic Framework

In situ infrared spectroscopy is an inexpensive, highly sensitive, and selective valuable tool to investigate the interaction of polycrystalline solids with adsorbates. Vibrational spectra provide information on the chemical nature of adsorbed species and their structure. Thus, they are very useful for obtaining molecular level understanding of surface species. The IR spectrum of the sample itself gives some direct information about the material. General conclusions can be drawn concerning hydroxyl groups, some stable surface species and impurities. However, the spectrum of the sample is &#34;blind&#34; with respect to the presence of coordinatively unsaturated ions and gives rather poor information about the acidity of surface hydroxyls, species decisive for the adsorption and catalytic properties of the materials. Furthermore, no discrimination between bulk and surface species can be made. These problems are solved by the use of probe molecules, substances that interact specifically with the surface; the alteration of some spectral features of these molecules as a result of adsorption provides valuable information about the nature, properties, location, concentration, etc., of the surface sites.
The experimental protocol for in-situ IR studies of gas/sample interaction includes preparation of a sample pellet, activation of the material, initial spectral characterization through the analysis of the background spectra, characterization by probe molecules, and study of the interaction with a particular set of gas mixtures. In this paper we investigate a zirconium terephthalate metal organic framework, Zr6O4(OH)4(BDC)6 (BDC = benzene-1,4-dicarboxylate), namely UiO-66 (UiO refers to University of Oslo). The acid sites of the UiO-66 sample are determined by using CO and CD3CN as molecular probes. Furthermore, we have demonstrated that CO2 is adsorbed on basic sites exposed on dehydroxylated UiO-66. Introduction of water to the system produces hydroxyl groups acting as additional CO2 adsorption sites. As a result, CO2 adsorption capacity of the sample is strongly enhanced.

In situ FTIR Spectroscopy as a Tool for Investigation of Gas/Solid Interaction: Water-Enhanced CO2 Adsorption in UiO-66 Metal-Organic Framework

The use of FTIR spectroscopy for investigation of the surface properties of polycrystalline solids is described. Preparation of sample pellets, activation procedures, characterization with probe molecules and model studies of CO2 adsorption are discussed.

In situ infrared spectroscopy is an inexpensive, highly sensitive, and selective valuable tool to investigate the interaction of polycrystalline solids ...