Name: preparation of highly porous coordination polymer coatings on macroporous polymer monoliths for enhanced enrichment of phosphopeptides
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Description: Watch this Scientific Journal Video about Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides at JoVE.com

This work has been performed at the Molecular Foundry, Lawrence Berkeley National Laboratory and supported by the Office of Science, Office of Basic Energy Sciences, Scientific User Facilities Division of the US Department of Energy, under Contract No. DE-AC02&#8211;05CH11231. The financial support of F.M. by a ME-Fulbright fellowship and A.S. by Higher Education Commission of Pakistan are gratefully acknowledged.

NOT: Başlamadan önce, tüm ilgili malzeme veri sayfaları (MSDS) kontrol edin. Sentetik ve uygulama prosedürleri kullanılan kimyasalların çeşitli toksik değildir. Tüm uygun güvenlik uygulamalarını takip ve yeterli koruyucu ekipman (laboratuvar önlüğü, tam uzunlukta pantolon, kapalı-toe ayakkabıları, koruyucu gözlük, eldiven) kullanın. Azot adsorpsiyon ölçümleri için sıvı azot (izolasyonlu eldiven, yüz maskesi) işlerken tüm kriyojenik kişisel koruyucu donanımları kullanın. <p class=...

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Orijinal polimerin monolit metaller bağlanabilen karboksilik fonksiyonel grupları içerir. Orijinal malzeme başlangıç ​​metal sitelerini koordine bir mikro-gözenekli bir ağ şekillendirme ek metal sitelerinin bir dizi içeren bir PCP kaplama (Şekil 1A) büyümek edebiliyoruz. Bu durum, hareketsiz metal iyonu yakınlık kromatografisi (IMAC) tekniği olarak metal türleri söz konusu ekstraksiyon ve saflaştırma işlemleri için çekici bir sunulan MOPH malzemeleri sağlar. Phosphopeptides z...

Gözenekli bir koordinasyon polimerler (yaratanlar) amorf ya da 1-3 kristalize olabilen 1, 2 ya da 3 boyutlu olarak uzanan bir koordinasyon kişiler tekrarlayan organik ligandlar ile bağlantılı metaller merkezlerine göre koordinasyon bileşikleri bulunmaktadır. Son yıllarda, gözenekli malzemelerin bu sınıf nedeniyle yüksek gözeneklilik, geniş kimyasal Ayarlanabilirliğin ve onların istikrar geniş ilgi gördü. Yaratanlar gaz depolama, gaz ayırma ve kataliz 3-6, ve çok yakın zamanda, yaratanlar ilk analitik uygulamalar 7 tarif edilmiştir dahil uygulamaları bir dizi için araştırılmıştır. Çünkü onların gelişmiş kimyasal işlevsellik ve yüksek gözenekli yaratanlar arıtma süreçleri ve kromatografik ayırımlar iyileştirilmesi için onların büyük potansiyeli hedef seçilmişlerdir, ve bu konuyu ilgili raporların bir numara 7-13 yayınlandı. Bununla birlikte, yaratanlar performansı, bir equivale şu anda değil,nedeniyle parçacıkların ya da kristallerin kendi tipik düzensiz şekilli morfolojiler nedeniyle bu katıların dolu yatak büyük parçacıklar arası boşluklar aracılığıyla hızlı difüzyon olasılığı mevcut kromatografik malzemeleri ile nt seviyesinde. Bu, düzensiz olarak dağıtılmış ambalaj dan daha düşük bir beklenen performans, hem de yüksek sütun backpressuresin ve istenmeyen pik şekli morfolojileri 14,15 yol açar. Parçacık arası boşluklara sayesinde hızlı yayılma sorunu çözmek ve eş zamanlı olarak analiz uygulamaları için yaratanlar performansını artırmak amacıyla, makro-yüzeyinde PCP ihtiva eden bir makro-gözenekli bir polimer monolit 16 dayanan bir hibrid malzemeden gelişimi olur istenebilecektir. Polimer yekpare keçeleri boncuk ve başarıyla birkaç c piyasaya sürülmüş en verimli alternatiflerden birini onları yapar, kendi gözenekler aracılığıyla konvektif akışını sürdürmek, tek parça malzemeleri kendine yeten<html> ompanies 17,18. Gözenekli polimer yekpare genellikle monomerinin polimerizasyonu ve tipik olarak organik çözücülerin ikili karışımlarıdır porogens, mevcudiyetinde bir çapraz bağlayıcı dayanmaktadır. Elde edilen monolitik malzemeler microglobular yapısı ve yüksek gözeneklilik ve akış geçirgenliğine sahiptir. Basit bir yaklaşım PCP içeren bir polimer monolit monolit polimerizasyon karışımı olarak sentezlenmiş yaratanlar doğrudan ilave dayanmaktadır hazırlamak için bu malzemeleri birleştirmek için. Yaratanlar sonuçlandı Bu yaklaşım çoğunlukla nihai malzemenin 14,15 daha fazla uygulama için aktif olan bir polimer iskele içinde gömülü değil. Bir farklı sentetik yaklaşımı, örneğin, kristal içinde bulunan gözeneklerin büyük bir kısmı bir polimer yekpare makro-erişilebilen yaratanlar, ya da kristal metal organik çerçevelerin (MOFs) üniform filmler geliştirmek için gereklidir. t &quot;&gt; Bu yazıda kolayca uygulanabilir yaratanlar bağlanması için uygun bir fonksiyonel grup, bir makro-gözenekli bir polimer destek üzerine dayanan bir metal-organik bir polimer karma malzemesi (MOPH) hazırlanması için bir protokol rapor kendi kendine yeten bir tek akış uygulamaları için optimum özelliklere sahip bir sütun biçiminde parça Takımı polimer monolit. polimer sentezi prosedürü basit bir oda sıcaklığı çözüm tabanlı takip eder &#160; yöntem, monolit 19-20 gözeneklerinin iç yüzeyi üzerinde bir PCP kaplama büyümesi. İlk örnek olarak, bir makro-gözenekli poli (stiren-divinilbenzen-metakrilik asit) yekpare olan, bir demir (III) benzenetricarboxylate (FeBTC) koordinasyon polimer filmin hazırlanmasını tarif etmektedir. Bu yöntem toplu tozlar hazırlanması gibi kapiler sütun için etkili olan ve tarif edilen protokol, diğer yaratanlar kolayca uygulanabilir değildir. Akış Throu fonksiyonel malzemeler olarak MOPHs potansiyelinin bir örnek olarakbu tip uygulamaların biz merkezleri Fe Phosphopeptides bağlanma afinitesini istismar sindirilmiş protein karışımları arasından fosfopeptidler zenginleştirmek (III) Fe yoğun bir kaplama içeren geliştirilmiş FeBTC MOPH uygulanan (III). geliştirilen protokol 21 üç ana bölümden oluşmaktadır: makropor organik polimer monolit destek hazırlanması; monolit gözeneklerin yüzeyinde PCP kaplama büyümesi; Phosphopeptides zenginleştirilmesi için uygulama.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Polyimide-coated capillaries</td>
			<td>Polymicro Technologies</td>
			<td>TSP100375</td>
			<td>100 &#956;m i.d.</td>
		</tr>
		<tr>
			<td>3-(trimethoxysilyl)propyl methacrylate, 98%</td>
			<td>Sigma-Aldrich</td>
			<td>440159</td>
			<td></td>
		</tr>
		<tr>
			<td>Styrene, 99%</td>
			<td>Sigma-Aldrich</td>
			<td>W323306</td>
			<td>Technical grade</td>
		</tr>
		<tr>
			<td>Divinylbenzene, 80%</td>
			<td>Sigma-Aldrich</td>
			<td>414565</td>
			<td></td>
		</tr>
		<tr>
			<td>Methacrylic acid, 98%</td>
			<td>Mallinckrodt</td>
			<td>MK150659</td>
			<td></td>
		</tr>
		<tr>
			<td>Toluene, &#8805;99.5%</td>
			<td>EMD chemicals</td>
			<td>MTX0735-6</td>
			<td></td>
		</tr>
		<tr>
			<td>Isooctane, &#8805;99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>650439</td>
			<td></td>
		</tr>
		<tr>
			<td>2,2&#39;-azobisisobutyronitrile, 98%</td>
			<td>Sigma-Aldrich</td>
			<td>441090</td>
			<td></td>
		</tr>
		<tr>
			<td>Aluminium oxide (basic alumina)</td>
			<td>Sigma-Aldrich</td>
			<td>199443</td>
			<td></td>
		</tr>
		<tr>
			<td>Iron (III) chloride hexahydrate, 97%</td>
			<td>Sigma-Aldrich</td>
			<td>236489</td>
			<td></td>
		</tr>
		<tr>
			<td>1,3,5-benzenetrycarboxylic acid, 95%</td>
			<td>Sigma-Aldrich</td>
			<td>482749</td>
			<td></td>
		</tr>
		<tr>
			<td>Acetonitrile, &#8805;99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>360457</td>
			<td></td>
		</tr>
		<tr>
			<td>Ammonium bicarbonate, &#8805;99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>9830</td>
			<td></td>
		</tr>
		<tr>
			<td>Trifluoroacetic acid, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>302031</td>
			<td></td>
		</tr>
		<tr>
			<td>Ethanol, &#8805;99.8%</td>
			<td>Sigma-Aldrich</td>
			<td>2854</td>
			<td></td>
		</tr>
		<tr>
			<td>Iodoacetamide, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>I1149</td>
			<td></td>
		</tr>
		<tr>
			<td>Dithiothreitol, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>43819</td>
			<td></td>
		</tr>
		<tr>
			<td>Monobasic sodium phosphate dihydrate, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>71505</td>
			<td></td>
		</tr>
		<tr>
			<td>Dibasic sodium phosphate dihydrate, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>71643</td>
			<td></td>
		</tr>
		<tr>
			<td>Phosphoric acid, &#8805;85%</td>
			<td>Sigma-Aldrich</td>
			<td>438081</td>
			<td></td>
		</tr>
		<tr>
			<td>2,5-dihydroxybenzoic acid, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>85707</td>
			<td></td>
		</tr>
		<tr>
			<td>Trypsin</td>
			<td>Sigma-Aldrich</td>
			<td>T8003</td>
			<td>Bovine pancreas</td>
		</tr>
		<tr>
			<td>&#946;-casein</td>
			<td>Sigma-Aldrich</td>
			<td>C6905</td>
			<td>Bovine milk</td>
		</tr>
		<tr>
			<td>ZipTip pipette tips</td>
			<td>Merck Millipore</td>
			<td>ZTC18S096</td>
			<td>C18 resin</td>
		</tr>
	</tbody>
</table>

preparation of highly porous coordination polymer coatings on macroporous polymer monoliths for enhanced enrichment of phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

Organik polimer yekpare gözenek yüzeyi üzerinde PCP büyüme şematik bir gösterimi, Şekil 1 &#39;de gösterilmiştir. Bu şekilde, bizim göstermektedir, ilk Fe (III) atomu karboksilik fonksiyonel gruplara koordine orijinal polimer yekpare gözenek yüzeyi üzerinde tutulan . Protokol izlenmek suretiyle, burada ek bir organik ligand ve tarif Fe (III) iyonları, polimer yekpare olan gözenekli bir koordinasyon ağ şekillendirme yüzeyine ilave edilir. Ayrıca, şematik akış geçiş destek olarak...

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Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

Phosphopeptides Gelişmiş Zenginleştirme için Makrogözenekli Polimer Monoliths üzerinde yüksek Gözenekli Koordinasyon Polymer Coatings Hazırlanması

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

Research

JoVE Journal

Chemistry

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