Yazarlar püskürtmeli kaplayıcı ekipmanları ile yardım için XRD spektrumları ve K. Booksh ile yaptığı yardım için Svilen Bobev teşekkür ederiz.

1. sentezi Ağacı benzeri ZnO / CdSSe Nanoyapılar <ol><li> Safir yüzeylerde tedavi öncesi ve altın kaplama Not: altın film ZnO nanotellerinin büyümesinde bir katalizör olarak hareket eder. <ol><li> sonikasyon 5 dakika ile% 99.5 etanol içinde temiz safir slaytlar (a-düzlemi, 10 x 10 x 1 mm) Au püskürtme için alt-tabaka hazırlanır. </li><li> Bir püskürtmeli kaplayıcı ve altın hedefi safir Slaytlarınıza 10 nm (± 2 nm) altın um kalınlığındaki bir film oluşturur. </li></ol></li><li> ZnO nanotellerinin sentezi NOT: Sonication adımı homojen bir ZnO 1.2.2 sonuçları ve karbon (ZnO / C) karışımı. Karıştırma işleminden sonra, karışım, gri bir renge dönüşür. sıkıştırma basamağı 1.2.3 hava karışımı içinde ve ZnO ve karbon yakın temas içinde olduğu, mevcut olmasını sağlar. CVD sonra ZnO nanotellerinin beyaz film tarafı aşağı tekneye doğru bakan, alt-tabaka üzerinde biriken olmalıdır. <ol><li> ZnO NANOPOWDER ve activ 1 g karıştırınbir- C (50:50 kütle payı), 10 mi% 99.5 etanol içinde bir spatula ile iyice karıştırın. </li><li> 30 dakika boyunca 20 ° C&#39;de bir su banyosu içinde sonikasyon karışımı, ve daha sonra 80 ° C&#39;de ~ 5 saat için bir fırın içinde kurutun. </li><li> Bir alümina tekne ZnO / C karışımı yerleştirin ve bir spatula ile iyice kompakt. </li><li> altın kaplamalı yüzü aşağı bakacak şekilde, alümina tekne üstünde altın kaplı safir slaytlar yerleştirin. Bir yatay borulu fırında kuvars tüpün merkezinde alümin tekne yerleştirin. </li><li> Oda sıcaklığında 40 sccm&#39;lik (RT) &#39;in bir akış oranında Ar ile 1 saat süre ile kuvars tüp temizleyin. 80 ° C / dakikalık bir hızda 900 ° C oda sıcaklığında, sıcaklık artışları ve argon akış hızı sabit tutulması. </li><li> 2 saat 900 ºC sıcaklık tutun. lastik tıpa gaz girişleri kaldırarak her iki ucunda kuvars tüp açın ve hava reaksiyonu için oksijen sağlamak için tüp girelim. </li><li> ru olan 3 saat 900 ° C reaksiyon sıcaklığı tutmakgrafik çubuklarıyla bBER stoperler kaldırıldı. 10 ° C / dk&#39;lık bir hızda oda sıcaklığına soğutun. </li><li> tekne ve fırının dışına slayt atın. </li></ol></li><li> ZnO nanotellerin üzerinde CdSSe şube Biriktirme NOT: CdS alümina tekne / Se merkezinde kuvars tüp sergilendi. hazırlanan ZnO nanoteller yukarı bakacak ve tekne 10 cm aşağı idi. bu ikinci CVD sonra ZnO / CdSSe nano bir sarı / portakal rengi bir film, bir slayt üzerine aktarılır. <ol><li> CdS ve CdSe (CdS / Se) toz kuyu (50:50 kütle fraksiyonu) 0.5 g karıştırın ve bir alümina tekne karışımı yerleştirin. iyi karışımı sıkıştırmak. </li><li> CdS / Se alümina tekne ve kuvars tüp içinde önceden hazırlanmış ZnO nanotel örnek yerleştirin. </li><li> 1 saat boyunca oda sıcaklığında 40 sccm&#39;lik bir akış oranında Ar ile tüp temizleyin. 80 ° C / dakikalık bir hızda 820 ° C reaksiyon sıcaklığını arttırır. 30 dakika boyunca 820 ° C&#39;de sıcaklık tutun. </li><li> de RT kadar soğumasını10 ° C / dk&#39;lık bir oranı. tekne ve fırının dışına slayt atın. </li></ol></li><li> ZnO ve CdSSe nanotellerin: Kontrol örneklerinin sentezi <ol><li> Aynı deneysel koşullar altında Bölüm 1.2&#39;de olduğu gibi ZnO nanoteller sentez. </li><li> CdS ve CdSe kompozisyon aynı miktarda, aynı deney koşulları altında, bölüm 1.3 gibi CdSSe nanoteller sentez, ancak bunun yerine ZnO-yatırılır slayt substrat olarak temiz, altın kaplı safir slayt. </li></ol></li></ol> 2. Morfolojik ve Kristalografik Karakterizasyonu <ol><li> Bir kelepçe ile SEM sahnede örnek monte edin ve SEM enstrüman vakum odasında numuneyi yerleştirin. 3 kV gerilimde 12,0 mm çalışma mesafesi ve 3000X defa ve 10,000X 11,12 arasında bir büyütme ile yüksek çözünürlüklü modu SEM görüntüleri çekmek. </li><li> Aynı çalışma mesafesi X-ışını detektörü kullanarak aynı numune ile EDS veri almak12.0 mm. Analiz moduna aleti ayarlayın ve 20-40 uA 13 bir akım ile sonuçlanan 20 kV voltaj ayarlayın. </li><li> Süzüldü Cu Ka radyasyonu (λ = 1,5418 Â), 11,12 kullanan bir X-ışını toz difraktometresi ile XRD spektrumu toplayın. </li></ol> 3. PL Emisyon Spektroskopisi ve Zaman çözülmesi PL Ömür Ölçümleri Not: PL spektrumu ve zaman dekorele tek foton sayma oda sıcaklığında (TCSPC) ölçümleri, bir Ti güçlendirilmiş kullanılarak gerçekleştirilmiştir: 400 nm dalga boyunda merkezli 50 FSEC puls dizileri üreten ikinci harmonik üretimi (SHG) sonra, safir osilatörün ve 1.76 bir çıkış gücü mW 14. <ol><li> lazer kadar ve dedektör örnek yüzünü konumlandırır örnek tutucu içine örnek sabitleyin. örnek üzerinde odaklanmak için lazer hizalama. fiber spektrometresi kullanılarak 900 nm dalga boylarında 500 nm numunelerin PL emisyon spektrumları ölçün. </li><li> (Ava tek foton dedektörü kullanınlanche foto diyot veya phototube) bir renkli cam filtre ve 500- veya 650-nm parazit bant geçiren filtreli zamana bağımlı PL ömürleri ölçmek için. </li><li> Ekle ZnO, CdSSe veya ZnO / CdSSe numune tutucu içine kayar. 500 nm bant geçiş filtresi ve 650 nm bant geçiş filtresi ile CdSSe veya ZnO / CdSSe örnekleri ile saf ZnO nanoteller ölçün. </li><li> Zaman çözünürlüklü floresan bozunma ömürleri ölçmek için bir zaman dekorele tek foton sayacı ya da hızlı osiloskop kullanın. </li></ol>

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Bu makaledeki veriler ve rakamlar Li ve ark., 17 ile nanoteknoloji literatürden zikrediliyor.

ZnO nanotellerin (kaynaklanıyor) dikey hizalama alt tabaka üzerinde epitaksiyel büyüme dayanmaktadır. ZnO nanotellerdir safir 12 bir düzlem periyodu ile eşleşir &lt;0001&gt; yönünde tercihen büyür. Bu nedenle, tipi ve alt-tabaka kalitesi çok önemlidir. 5 nm ile 20 ila tabaka üzerinde altın kaplama, farklı kalınlıklarda, test edilmiş ve ZnO nanotellerinin büyümesinde anlamlı bir farklılık göstermiştir edilmiştir. ZnO nanotellerinin uzunluğu kullanılır ZnO / C karışımı, Ar ak?...

ZnO 3.3 eV bir bant boşluk (BG), bir yüksek elektron hareketliliği ve büyük exciton bağlama enerjili 1,2 özelliklerine sahip II-VI yarı iletkendir. Optik cihazlar mevcut ve gelecekteki uygulamalar, güneş pilleri ve fotokataliz bir bolluk ile bol yarı iletken malzemedir. Bununla birlikte, ZnO görünür spektral aralıkta uygulanmasını sınırlar saydamdır. Bu nedenle, dar aralık yarı iletkenler 3, boya molekülleri 4 ve ışığa hassas polimerlere 5 olarak görünür ışık emici malzemeler, genellikle görülebilir ışık emilimi ZnO duyarlı için kullanılmıştır. CdS (BG 2.43 eV) ve CdSe (BG 1.76 eV) ortak II-VI dar aralık yarı iletkenler ve yoğun incelenmiştir. Üçlü alaşım CdSSe BG ve kafes parametreleri VI bileşenlerine 6,7 mol oranları değiştirilerek ayarlanabilir. ZnO / CdSSe nanokompozitler etkin photov sonuçlandığı bildirilmiştiroltaic enerji dönüşümü 8,9. CdSSe şube gelişmiş görünür ışık emilimi ile bir alt tabakaya doğru dikey olarak hizalanmış ZnO nanotellerinin verimli elektron taşıma yolu birleştiren gövde ve dallar 9,10 arasında etkin elektron transferi yol açtı. Böylece, dikey olarak hizalanmış ZnO nanoteller CdSSe dalları ile dekore edilmiştir, yeni bir ağaç gibi ZnO / CdSSe nano yapısını, sentezlenmiş. Bu kompozit malzeme, yeni güneş enerjisi dönüşüm cihazları için bir yapı bloğu olarak hareket edebilir. Bu protokol, ZnO nanotel dizileri, daha önce 11 yayınlanmış olan bir prosedür takip edilerek ZnO ve Cı tozlardan tek aşamalı bir kimyasal buhar biriktirme (CVD) ile bir safir alt-tabaka üzerinde yetiştirilen açıklamaktadır. ZnO nanotellerinin büyümesinin ardından, CVD ikinci aşama ZnO nanotellerin üzerinde CdSSe dalları büyümeye kullanılır. Bu X-ışını toz difraksiyonu (XRD), taramalı elektron mikroskobu (SEM) ve istihdamEnerji dağılımlı X-ışını spektroskopisi (EDS) ZnO / CdSSe nanotrees (NTS) kristal yapıları, morfolojisi ve bileşimini ölçmek için. şube ve kök arasındaki optik özellikleri ve yük taşıyıcı transfer mekanizması fotolüminesans (PL) spektroskopisi ve zamana bağımlı PL ömür boyu ölçümleri ile incelenmiştir.

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>ZnO</td>
			<td>Sigma Aldrich</td>
			<td>1314-13-2</td>
			<td></td>
		</tr>
		<tr>
			<td>Activated Carbon</td>
			<td>Alfa</td>
			<td>231-153-3</td>
			<td></td>
		</tr>
		<tr>
			<td>CdSe</td>
			<td>Sigma Aldrich</td>
			<td>1306-24-7</td>
			<td></td>
		</tr>
		<tr>
			<td>CdS</td>
			<td>Sigma Aldrich</td>
			<td>1306-23-6</td>
			<td></td>
		</tr>
		<tr>
			<td>Sapphire</td>
			<td>MTI</td>
			<td>2SP</td>
			<td>a-plane, 10 &#215; 10 &#215; 1 mm</td>
		</tr>
		<tr>
			<td>Furnace</td>
			<td>Lindberg Blue M</td>
			<td>SSP</td>
			<td></td>
		</tr>
		<tr>
			<td>Scanning electron microscope</td>
			<td>Hitachi</td>
			<td>S5700</td>
			<td>assembled with an Oxford Inca X-act detector</td>
		</tr>
		<tr>
			<td>X-ray powder diffractometer&#160;</td>
			<td>Rigaku&#160;</td>
			<td>MiniFlex</td>
			<td>filtered Cu K&#945; radiation (&#955;=1.5418 &#197;)</td>
		</tr>
		<tr>
			<td>Amplified Ti:sapphire oscillator&#160;</td>
			<td>Coherent Mantis</td>
			<td>Coherent Legend-Elite</td>
			<td></td>
		</tr>
		<tr>
			<td>Single photon detection module&#160;</td>
			<td>ID Quantique</td>
			<td>ID-100</td>
			<td></td>
		</tr>
		<tr>
			<td>Sputter coater</td>
			<td>Cressington</td>
			<td>308</td>
			<td>assembled with gold target</td>
		</tr>
		<tr>
			<td>Fiber probe spectrometer</td>
			<td>Photon Control</td>
			<td>SPM-002</td>
			<td></td>
		</tr>
		<tr>
			<td>Colored Glass Filter</td>
			<td>Thorlabs</td>
			<td>FGB37-A - &#216;25 mm BG40</td>
			<td>AR Coated: 350 - 700 nm&#160;</td>
		</tr>
		<tr>
			<td>Compressed argon gas</td>
			<td>Keen</td>
			<td>7440-37-1</td>
			<td></td>
		</tr>
	</tbody>
</table>

synthesis of hierarchical zno/cdsse heterostructure nanotrees

İki aşamalı bir kimyasal buhar depozisyon yöntemi Burada ağaç gibi hiyerarşik ZnO / CdSSe hetero nano hazırlamak için kullanılır. yapılar dikey şeffaf safir alt tabaka üzerine hizalanmış ZnO nanotellerin yetiştirilen CdSSe şube oluşmaktadır. morfoloji taramalı elektron mikroskobu ile ölçüldü. Kristal yapı, X-ışını toz difraksiyon analizi ile belirlendi. Hem ZnO kök ve CdSSe dalları ağırlıklı olarak hekzagonal kristal yapıya sahiptir. CdSSe dallarında S ve Se mol oranı enerji dispersif X-ışını spektroskopi ile ölçülmüştür. CdSSe dalları mutlaka görülebilir ışık emilmesi ile sonuçlanır. Fotolüminesans (PL) spektroskopisi kök ve dalları bir tip-II heteroeklem oluşturduğunu gösterdi. Bireysel ZnO gelen emisyon kaynaklanıyor ya da CdSSe şubeleri ile karşılaştırıldığında ve CdSSe ve ZnO arasındaki hızlı şarj transferini işaret ettiği PL ömür boyu ölçümleri ağaçlardan emisyon ömrü bir azalma olduğunu gösterdi. vertiCally&#39;nin hizalanmış ZnO substrata doğrudan elektron taşıma yolu sağlar ve görünür ışık photoexcitation sonrası etkili ücreti ayrımına izin kaynaklanmaktadır. Yukarıda belirtilen özelliklerin kombinasyonu ZnO / CdSSe güneş hücreleri, fotokataliz ve opto elektronik cihazlarda uygulamalar için umut verici adaylar nanotrees yapar.

Şekil 1 ZnO / CdSSe NTS büyüme mekanizmasını göstermektedir. prosedür katalitik olmayan buhar-katı (VS) büyüme takiben katalitik buhar-sıvı-katı (VLS) sürecini içermiştir. İlk VLS adımda, ZnO ve Cı metal Zn ve karbon oksit ile sonuçlanan, Ar atmosferde reaksiyona girmektedir. Zn, daha sonra safir alt-tabaka üzerinde altın ön içinde eritilir. ZnO nanoteller çözünmüş Zn ve kalıntı oksijen büyür. İkinci aşamada, kısa bir ZnO tohumları ü...

Watch this Scientific Journal Video about Synthesis of Hierarchical ZnO/CdSSe Heterostructure Nanotrees at JoVE.com

Synthesis of Hierarchical ZnO/CdSSe Heterostructure Nanotrees

Burada, CdSSe dalları dikey olarak hizalanmış ZnO nanotellerin yetiştirilen yeni ağaç benzeri hiyerarşik ZnO / CdSSe nano hazırlamak ve karakterize eder. Ortaya çıkan nanotrees güneş enerjisi dönüşüm ve diğer opto-elektronik cihazlar için potansiyel bir malzemedir.

Hiyerarşik ZnO / CdSSe Heteroyapı Nanotrees sentezi

A two-step chemical vapor deposition procedure is here employed to prepare tree-like hierarchical ZnO/CdSSe hetero-nanostructures. The structures are ...

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9.9K Görüntüleme.  University of Delaware.  Burada, CdSSe dalları dikey olarak hizalanmış ZnO nanotellerin yetiştirilen yeni ağaç benzeri hiyerarşik ZnO / CdSSe nano hazırlamak ve karakterize eder. Ortaya çıkan nanotrees güneş enerjisi dönüşüm ve diğer opto-elektronik cihazlar için potansiyel bir malzemedir. 

Video: Synthesis of Hierarchical ZnO/CdSSe Heterostructure Nanotrees

Synthesis of Immunotargeted Magneto-plasmonic Nanoclusters

Magnetic and plasmonic properties combined in a single nanoparticle provide a synergy that is advantageous in a number of biomedical applications including contrast enhancement in novel magnetomotive imaging modalities, simultaneous capture&#160;and detection of circulating tumor cells (CTCs),&#160;and multimodal molecular imaging combined with photothermal therapy of cancer cells. These applications have stimulated significant interest in development of protocols for synthesis of magneto-plasmonic nanoparticles with optical absorbance in the near-infrared (NIR) region and a strong magnetic moment. Here, we present a novel protocol for synthesis of such hybrid nanoparticles that is based on an oil-in-water microemulsion method. The unique feature of the protocol described herein is synthesis of magneto-plasmonic nanoparticles of various sizes from primary blocks which also have magneto-plasmonic characteristics. This approach yields nanoparticles with a high density of magnetic and plasmonic functionalities which are uniformly distributed throughout the nanoparticle volume. The hybrid nanoparticles can be easily functionalized by attaching antibodies through the Fc moiety leaving the Fab portion that is responsible for antigen binding available for targeting.

Here, we describe a protocol for synthesis of magneto-plasmonic nanoparticles with a strong magnetic moment and a strong near-infrared (NIR) absorbance. The protocol also includes antibody conjugation to the nanoparticles through the Fc moiety for various biomedical applications which require molecular specific targeting.

Immunotargeted sentezi Magneto-plasmonik nanoklastırlar

Magnetic and plasmonic properties combined in a single nanoparticle provide a synergy that is advantageous in a number of biomedical applications ...

Kimya

Synthesis and Characterization of Functionalized Metal-organic Frameworks

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy.

Synthesis, activation, and characterization of intentionally designed metal-organic framework materials is challenging, especially when building blocks are incompatible or unwanted polymorphs are thermodynamically favored over desired forms. We describe how applications of solvent-assisted linker exchange, powder X-ray diffraction in capillaries and activation via supercritical CO2 drying, can address some of these challenges.

Fonksiyonlu Sentezi ve Karakterizasyonu Metal-organik Altyapıları

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and ...

Synthesis of Indoxyl-glycosides for Detection of Glycosidase Activities

Indoxyl glycosides proved to be valuable and versatile tools for monitoring glycosidase activities. Indoxyls are released by enzymatic hydrolysis and are rapidly oxidized, for example by atmospheric oxygen, to indigo type dyes. This reaction enables fast and easy screening in vivo without isolation or purification of enzymes, as well as rapid tests on agar plates or in solution (e.g., blue-white screening, micro-wells) and is used in biochemistry, histochemistry, bacteriology and molecular biology. Unfortunately the synthesis of such substrates proved to be difficult, due to various side reactions and the low reactivity of the indoxyl hydroxyl function. Especially for glucose type structures low yields were observed. Our novel approach employs indoxylic acid ester as key intermediates. Indoxylic acid esters with varied substitution patterns were prepared on scalable pathways. Phase transfer glycosylations with those acceptors and peracetylated glycosyl halides can be performed under common conditions in high yields. Ester cleavage and subsequent mild silver mediated glycosylation yields the peracetylated indoxyl glycosides in high yields. Finally deprotection is performed according to Zempl&#233;n.

Indoxyl glycosides are well-established and widely used tools for enzyme screening and enzyme activity monitoring. Especially for glucose type structures previous syntheses proved to be challenging and low yielding. Our novel approach employs indoxylic acid esters as precious intermediates to yield a considerable number of indoxyl glycosides in good yields.

Glikosidaz Faaliyetlerinin Belirlenmesi için indoksil-glikozitler sentezi

Indoxyl glycosides proved to be valuable and versatile tools for monitoring glycosidase activities. Indoxyls are released by enzymatic hydrolysis and are ...

Synthesis and Characterization of Supramolecular Colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical properties for applications in photonics, drug delivery and coating technology. Here we present a new family of colloidal building blocks, coined supramolecular colloids, whose self-assembly is controlled through surface-functionalization with a benzene-1,3,5-tricarboxamide (BTA) derived supramolecular moiety. Such BTAs interact via directional, strong, yet reversible hydrogen-bonds with other identical BTAs. Herein, a protocol is presented that describes how to couple these BTAs to colloids and how to quantify the number of coupling sites, which determines the multivalency of the supramolecular colloids. Light scattering measurements show that the refractive index of the colloids is almost matched with that of the solvent, which strongly reduces the van der Waals forces between the colloids. Before photo-activation, the colloids remain well dispersed, as the BTAs are equipped with a photo-labile group that blocks the formation of hydrogen-bonds. Controlled deprotection with UV-light activates the short-range hydrogen-bonds between the BTAs, which triggers the colloidal self-assembly. The evolution from the dispersed state to the clustered state is monitored by confocal microscopy. These results are further quantified by image analysis with simple routines using ImageJ and Matlab. This merger of supramolecular chemistry and colloidal science offers a direct route towards light- and thermo-responsive colloidal assembly encoded in the surface-grafted monolayer.

A protocol for the synthesis and characterization of colloids coated with supramolecular moieties is described. These supramolecular colloids undergo self-assembly upon the activation of the hydrogen-bonds between the surface-anchored molecules by UV-light.

Supramoleküler Kolloidlerin Sentezi ve Karakterizasyonu

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

Hydroquinone Based Synthesis of Gold Nanorods

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the synthetic methods for the preparation of gold nanorods are still not fully optimized. In this paper we describe a new, highly efficient, two-step protocol based on the use of hydroquinone as a mild reducing agent. Our approach allows the preparation of nanorods with a good control of size and aspect ratio (AR) simply by varying the amount of hexadecyl trimethylammonium bromide (CTAB) and silver ions (Ag+) present in the "growth solution". By using this method, it is possible to markedly reduce the amount of CTAB, an expensive and cytotoxic reagent, necessary to obtain the elongated shape. Gold nanorods with an aspect ratio of about 3 can be obtained in the presence of just 50 mM of CTAB (versus 100 mM used in the standard protocol based on the use of ascorbic acid), while shorter gold nanorods are obtained using a concentration as low as 10 mM.

This paper describes a protocol for the synthesis of gold nanorods, based on the use of hydroquinone as reducing agent, plus the different mechanisms for controlling their size and aspect ratio.

Altın nanorods hidrokinon Esaslı Sentezi

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the ...

Synthesis and Mass Spectrometry Analysis of Oligo-peptoids

Peptoids are sequence-controlled peptide-mimicking oligomers consisting of N-alkylated glycine units. Among many potential applications, peptoids have been thought of as a type of molecular information storage. Mass spectrometry analysis has been considered the method of choice for sequencing peptoids. Peptoids can be synthesized via solid phase chemistry using a repeating two-step reaction cycle. Here we present a method to manually synthesize oligo-peptoids and to analyze the sequence of the peptoids using tandem mass spectrometry (MS/MS) techniques. The sample peptoid is a nonamer consisting of alternating N-(2-methyloxyethyl)glycine (Nme) and N-(2-phenylethyl)glycine (Npe), as well as an N-(2-aminoethyl)glycine (Nae) at the N-terminus. The sequence formula of the peptoid is Ac-Nae-(Npe-Nme)4-NH2, where Ac is the acetyl group. The synthesis takes place in a commercially available solid-phase reaction vessel. The rink amide resin is used as the solid support to yield the peptoid with an amide group at the C-terminus. The resulting peptoid product is subjected to sequence analysis using a triple-quadrupole mass spectrometer coupled to an electrospray ionization source. The MS/MS measurement produces a spectrum of fragment ions resulting from the dissociation of charged peptoid. The fragment ions are sorted out based on the values of their mass-to-charge ratio (m/z). The m/z values of the fragment ions are compared against the nominal masses of theoretically predicted fragment ions, according to the scheme of peptoid fragmentation. The analysis generates a fragmentation pattern of the charged peptoid. The fragmentation pattern is correlated to the monomer sequence of the neutral peptoid. In this regard, MS analysis reads out the sequence information of the peptoids.

A protocol is described for the manual synthesis of oligo-peptoids followed by sequence analysis by mass spectrometry.

Sentez ve kütle spektrometresi analizleri Oligo-peptoids

Peptoids are sequence-controlled peptide-mimicking oligomers consisting of N-alkylated glycine units. Among many potential applications, peptoids have ...

Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a challenge, as it requires asymmetric growth of symmetric crystals. Here, we report a distinctive synthesis of substrate-bound Au nanowires. This template-free synthesis employs thiolated ligands and substrate adsorption to achieve the continuous asymmetric deposition of Au in solution at ambient conditions. The thiolated ligand prevented the Au deposition on the exposed surface of the seeds, so the Au deposition only occurs at the interface between the Au seeds and the substrate. The side of the newly deposited Au nanowires is immediately covered with the thiolated ligand, while the bottom facing the substrate remains ligand-free and active for the next round of Au deposition. We further demonstrate that this Au nanowire growth can be induced on various substrates, and different thiolated ligands can be used to regulate the surface chemistry of the nanowires. The diameter of the nanowires can also be controlled with mixed ligands, in which another &#34;bad&#34; ligand could turn on the lateral growth. With the understanding of the mechanism, Au nanowire-based nanostructures can be designed and synthesized.

We report a solution-based method to synthesize substrate-bound Au nanowires. By tuning the molecular ligands used during the synthesis, the Au nanowires can be grown from various substrates with different surface properties. Au nanowire-based nanostructures can also be synthesized by adjusting the reaction parameters.

Substrat bağlı Au Nanowires bir aktif yüzey büyüme mekanizması yoluyla sentezi

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a ...

Solid-phase Synthesis of [4.4] Spirocyclic Oximes

A convenient synthetic route for spirocyclic heterocycles is well sought after due to the molecule&#39;s potential use in biological systems. By means of solid-phase synthesis, regenerating Michael (REM) linker strategies, and 1,3-dipolar cycloaddition, a library of structurally similar heterocycles, both with and without a spirocyclic center, can be constructed. The main advantages of the solid-support synthesis are as follows: first, each reaction step can be driven to completion using a large excess of reagents resulting in high yields; next, the use of commercially available starting materials and reagents keep the costs low; finally, the reaction steps are easy to purify via simple filtration. The REM linker strategy is attractive because of its recyclability and traceless nature. Once a reaction scheme is completed, the linker can be reused multiple times. In a typical solid-phase synthesis, the product contains either a part of or the whole linker, which can prove undesirable. The REM linker is &#34;traceless&#34; and the point of attachment between the product and the polymer is indistinguishable. The high diastereoselectivity of the intramolecular 1,3-dipolar cycloaddition is well documented. Limited by the insolubility of the solid support, the reaction progression can only be monitored by a change in the functional groups (if any) via infrared (IR) spectroscopy. Thus, the structural identification of intermediates cannot be characterized by conventional nuclear magnetic resonance (NMR) spectroscopy. Other limitations to this method stem from the compatibilities of the polymer/linker to the desired chemical reaction scheme. Herein we report a protocol that allows for the convenient production of spirocyclic heterocycles that, with simple modifications, can be automated with high-throughput techniques.

Here we present a protocol to demonstrate an efficient method for the synthesis of spirocyclic heterocycles. The five-step process utilizes solid-phase synthesis and regenerating Michael linker strategies. Generally difficult to synthesize, we present a customizable method for the synthesis of spirocyclic molecules otherwise inaccessible to other modern approaches.

Katı faz [4.4] Spirocyclic Oximes sentezi

A convenient synthetic route for spirocyclic heterocycles is well sought after due to the molecule&#39;s potential use in biological systems. By means of ...

Synthesis and Characterization of Amphiphilic Gold Nanoparticles

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of their interactions with cell membranes, lipid bilayers, and viruses. The hydrophilic ligands make these particles colloidally stable in aqueous solutions and the combination with hydrophobic ligands creates an amphiphilic particle that can be loaded with hydrophobic drugs, fuse with the lipid membranes, and resist nonspecific protein adsorption. Many of these properties depend on nanoparticle size and the composition of the ligand shell. It is, therefore, crucial to have a reproducible synthetic method and reliable characterization techniques that allow the determination of nanoparticle properties and the ligand shell composition. Here, a one-phase chemical reduction, followed by a thorough purification to synthesize these nanoparticles with diameters below 5 nm, is presented. The ratio between the two ligands on the surface of the nanoparticle can be tuned through their stoichiometric ratio used during synthesis. We demonstrate how various routine techniques, such as transmission electron microscopy (TEM), nuclear magnetic resonance (NMR), thermogravimetric analysis (TGA), and ultraviolet-visible (UV-Vis) spectrometry, are combined to comprehensively characterize the physicochemical parameters of the nanoparticles.

Amphiphilic gold nanoparticles can be used in many biological applications. A protocol to synthesize gold nanoparticles coated by a binary mixture of ligands and a detailed characterization of these particles is presented.

Amphiphilik altın nanopartiküller sentezi ve karakterizasyonu

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of ...

Hierarchical and Programmable One-Pot Oligosaccharide Synthesis

This article presents a general experimental protocol for programmable one-pot oligosaccharide synthesis and demonstrates how to use Auto-CHO software for generating potential synthetic solutions. The programmable one-pot oligosaccharide synthesis approach is designed to empower fast oligosaccharide synthesis of large amounts using thioglycoside building blocks (BBLs) with the appropriate sequential order of relative reactivity values (RRVs). Auto-CHO is a cross-platform software with a graphical user interface that provides possible synthetic solutions for programmable one-pot oligosaccharide synthesis by searching a BBL library (containing about 150 validated and &#62;50,000 virtual BBLs) with accurately predicted RRVs by support vector regression. The algorithm for hierarchical one-pot synthesis has been implemented in Auto-CHO and uses fragments generated by one-pot reactions as new BBLs. In addition, Auto-CHO allows users to give feedback for virtual BBLs to keep valuable ones for further use. One-pot synthesis of stage-specific embryonic antigen 4 (SSEA-4), which is a pluripotent human embryonic stem cell marker, is demonstrated in this work.

This protocol demonstrates how to use the Auto-CHO software for hierarchical and programmable one-pot synthesis of oligosaccharides. It also describes the general procedure for RRV determination&#160;experiments and one-pot glycosylation of SSEA-4.

Hiyerarşik ve Programlanabilir Tek Pot Oligosakkarit Sentezi

This article presents a general experimental protocol for programmable one-pot oligosaccharide synthesis and demonstrates how to use Auto-CHO software for ...