This study was supported by the grant from AACP New Pharmacy Faculty Research Award Program, Medical Research Foundation of Oregon New Investigator Grant, Oregon State University-Startup fund, and Pacific University, School of Pharmacy Start-up fund.

Çözücü döküm yöntemiyle ayrı ayrı ve Çok-ilaç yüklü misellerin hazırlanması 1. <ol><li> Çift ilaç miselleri için 1 mg her (DDM) de DTX 1 mg veya EVR 1 mg veya her ikisi ilaçlar tartılır. </li><li> PEG 2000 15 mg tartılır - -PLA 1800 veya PEG 4000 b - b -PLA 2200 bireysel ya da DDM biri için. </li><li> Ilaç / uyuşturucu ve bir 5 ml&#39;lik yuvarlak dipli bir şişeye asetonitril ve yerine 0.5 ml içindeki polimeri ayrıştırın. </li><li> Bir döner buharlaştırıcı kullanılarak indirgenmiş basınç altında ilaç (lar)-polimer asetonitril çözeltiyi buharlaştırarak ince ilaç dağıtılmış polimer film oluşturmak. 100 rpm, 40 o C su banyosu sıcaklığında ve 3 dakika daha 100 mbar, bir redüksiyon sonrasında 5 dakika boyunca 260 mbar&#39;lık bir vakum basıncı döner bir buharlaştıncı ayarlayın. </li><li> 50 ° C&#39;de iyonu giderilmiş su, 0.5 ml ilaç polimer film rehidrate ve yavaşça miseller oluşturmak için çalkalanır. </li><li> Filtre sonucu0.2 um naylon filtre vasıtasıyla misel çözeltisi ing 1,5 ml santrifüj tüpüne bir Erimemiş ilaç veya kirleri çıkarmak için. </li></ol> Ters fazlı yüksek performanslı sıvı kromatografisi (RP-HPLC) kullanarak Değerlendirme miseller ilaç yükleme ve stabilitesi 2. <ol><li> 1 ml / dk&#39;lık bir akış oranında, bir cep asetonitril / su fazı (62/38)% 0.1 fosforik asit,% 1 metanol ile izokratik modda, 40 ° C&#39;de equilibriated bir C8 sütunu ile RP-HPLC analizi gerçekleştirmek ve 10 ul bir enjeksiyon hacmi. </li><li> Önceden ilk ilaç yükleme belirlemek için RP-HPLC ile analiz mobil faz: 100 taze hazırlanmış miseller (bölüm 1) 1 seyreltin. RP-HPLC ile tekrar değerlendirilmesi ve 24 saat boyunca miselleri içine ilaç (lar) dengesini belirlemek için mobil faz olarak 100 seyreltilmiş örnekleri: Mağaza seyreltilmemiş bağımsız miselleri ve 48 st için oda sıcaklığında (25 ° C) de DDM ve taze 1 hazırlar. </li><li> Sırasıyla 227 ve 279 nm DTX ve EVR doruklarına Monitörsırasıyla 1.7 ve 5.7 dakika tutma süreleri ile. Üçlü olarak tüm ölçümleri yapın. Ortalama ± SD ilaç yüklemesi olarak mevcut veriler. </li></ol> Dinamik ışık saçılımı ile misel Partikül Boyutu 3. Değerlendirmesi (DLS) <ol><li> 1.5 mg / ml&#39;lik nihai bir polimer konsantrasyonuna vermek üzere 1:20 oranında iyonu giderilmiş su içinde (bölüm 1 &#39;de tarif edildiği gibi), taze hazırlanmış miseller seyreltilir. </li><li> Saçılma belirlemek için 173 ° He-Ne lazer (633 nm) yoğunluğunu ölçün. 2 dakika süresince ön-dengeyi takiben 25 ° C &#39;de, tüm ölçümler gerçekleştirmek. </li><li> Üçlü olarak tüm ölçümleri yapın. Dağıtım polidispersite indeksi (PDI) ile birlikte SD ± Ortalama Z-ortalama boyutu olarak mevcut veriler. </li></ol> Bireysel miselleri ve DDM 4. Değerlendirme In Vitro İlaç Yayın <ol><li> 3 ml diyaliz kaseti içine bölüm 1. Yük misellerin 2.5 ml açıklandığı gibi bireysel miseller ve DDM hazırlayın7000 g / mol bir molekül ağırlığı kesme değeri (MWCO). Not: Bu MWCO kaset dışına serbestçe yaygın ve böylece lavabo koşulları sağlamak için ilişkilendirilmemiş polimer molekülleri ile birlikte ücretsiz ilaç (lar) etkinleştirmek için seçildi. </li><li> (Stok 200 mM&#39;lik çözelti seyreltilerek hazırlandı), 10 mM pH 7.4 fosfat tampon maddesi 2.5 L, kasetler yerleştirin ve lavabo koşulları temin etmek üzere bir tampon her 3 saat değiştirin. Deney süresi boyunca 37 o C tampon sıcaklığını muhafaza. </li><li> &#39;De 0, 0.5, 1, 2, 3, 6, 9, 12, 24, ve 48 saat, kasetlerinde çözeltisi 150 ul çekme ve taze tampon 150 ul ile değiştirin. </li><li> Ilaç konsantrasyonu belirlemek için 2. bölümünde kurulan RP-HPLC kullanılarak numunelerin analiz. Stastitical yazılımını kullanarak bir fazlı üstel dernek ile basit difüzyon modeline dayalı ilaç (lar) salım verileri Eğrisi-uyacak. </li><li> E ilaç salımı% 50 ulaşmak için gereken süreyi hesaplayın (t 1/2)eğri dayanan bireysel miseller veya DDM olarak ach uyuşturucu. Dördüzden tüm ölçümleri yapın. </li></ol>

<ol>
	<li>Yokoyama, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymeric+micelles+as+a+new+drug+carrier+system+and+their+required+considerations+for+clinical+trials.">Polymeric micelles as a new drug carrier system and their required considerations for clinical trials.</a> Expert Opin Drug Deliv. 7, 145-158 (2010).</li><li>Shin, H. C., Alani, A. W., Rao, D. A., Rockich, N. C., Kwon, G. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multi-drug+loaded+polymeric+micelles+for+simultaneous+delivery+of+poorly+soluble+anticancer+drugs.">Multi-drug loaded polymeric micelles for simultaneous delivery of poorly soluble anticancer drugs.</a> J Control Release. 140, 294-300 (2009).</li><li>Adams, M. L., Lavasanifar, A., Kwon, G. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Amphiphilic+block+copolymers+for+drug+delivery.">Amphiphilic block copolymers for drug delivery.</a> J Pharm Sci. 92, 1343-1355 (2003).</li><li>Oerlemans, C., 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=Polymeric+micelles+in+anticancer+therapy:+targeting,+imaging+and+triggered+release.">Polymeric micelles in anticancer therapy: targeting, imaging and triggered release.</a> Pharm Res. 27, 2569-2589 (2010).</li><li>Shin, H. C., 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=A+3-in-1+polymeric+micelle+nanocontainer+for+poorly+water-soluble+drugs.">A 3-in-1 polymeric micelle nanocontainer for poorly water-soluble drugs.</a> Mol Pharm. 8, 1257-1265 (2011).</li><li>Hasenstein, J. R., 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=Antitumor+activity+of+Triolimus:+a+novel+multidrug-loaded+micelle+containing+Paclitaxel+Rapamycin,+and+17-AAG.">Antitumor activity of Triolimus: a novel multidrug-loaded micelle containing Paclitaxel Rapamycin, and 17-AAG.</a> Mol Cancer Ther. 11, 2233-2242 (2012).</li><li>Mazzaferro, S., 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=Bivalent+sequential+binding+of+docetaxel+to+methyl-beta-cyclodextrin.">Bivalent sequential binding of docetaxel to methyl-beta-cyclodextrin.</a> Int J Pharm. 416, 171-180 (2011).</li><li>Iwase, Y., Maitani, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+and+in+vivo+evaluation+of+liposomal+everolimus+for+lung+carcinoma+and+thyroid+carcinoma.">Preparation and in vivo evaluation of liposomal everolimus for lung carcinoma and thyroid carcinoma.</a> Biol Pharm Bull. 35, 975-979 (2012).</li><li>Mishra, G. P., Doddapaneni, B. S., Nguyen, D., Alani, A. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Antiangiogenic+effect+of+docetaxel+and+everolimus+as+individual+and+dual-drug-loaded+micellar+nanocarriers.">Antiangiogenic effect of docetaxel and everolimus as individual and dual-drug-loaded micellar nanocarriers.</a> Pharm Res. 31, 660-669 (2014).</li><li>Xu, W., Ling, P., Zhang, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymeric+micelles,+a+promising+drug+delivery+system+to+enhance+bioavailability+of+poorly+water-soluble+drugs.">Polymeric micelles, a promising drug delivery system to enhance bioavailability of poorly water-soluble drugs.</a> J Drug Deliv. 2013, 340315 (2013).</li><li>Lavasanifar, A., Samuel, J., Kwon, G. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Poly(ethylene+oxide)-block-poly(L-amino+acid)+micelles+for+drug+delivery.">Poly(ethylene oxide)-block-poly(L-amino acid) micelles for drug delivery.</a> Adv Drug Deliv Rev. 54, 169-190 (2002).</li></ol>

The authors have nothing to disclose.

The use of polymeric micelles for drug delivery continues to expand due to their versatility and ability to deliver hydrophobic drugs for various disease states. Therefore, the techniques needed to prepare and characterize these formulations prior to use in cell culture or animals is a critical first step to determine the best pairing between the drug and the polymer. PEG-b-PLA are excellent amphiphilic block copolymers for drug delivery purposes. However, the block length of the hydrophilic and hydrophobic s...

Hidrofilik ve hidrofobik alanlardan oluşur yinelenen yapısına Amfifilik blok kopolimerleri kendiliğinden polimerik miseller olarak bilinen üç boyutlu bir makro-moleküler derlemeleri oluşturmak üzere kendi kendine birleşebilen olabilir. Bu yapılar, bir hidrofilik kabuk tarafından çevrelenmiş bir iç hidrofobik bir çekirdeğe sahiptir. Hidrofobik merkez fiziksel olarak yakalanmalarında hidrofobik etkileşimler yoluyla ya da polimer omurgasına kimyasal konjügasyon yoluyla hidrofobik ilaçların da kapsama alınması için yeteneği vardır. 1 Bir çok avantajı, ilacın verilmesi için miselleri meydana getirmek üzere, bu blok kopolimerleri kullanarak bulunmaktadır. Bu polimerlerin az çözünen ilaçların birleşme, dahil ilaçların farmakokinetik özelliklerini iyileştirmek ve biyo-uyumluluk ve / veya biyo-bozunabilirlik içerir olanağına klasik çözünür hale güvenli bir alternatif yapar. 2, polimerik miseller kullanmanın bir diğer avantajı 15- arasında kendi kolloidal parçacık büyüklüğü olan pa için onları çekici hale 150 nm 3,eksipiyanlar teslimat. Bu nedenle, son 20 yılda, polimerik miseller, özellikle kanser terapisi için suda zayıf çözünür ilaçlar için uygun bir ilaç verme sistemleri olarak ortaya çıkmıştır. 3,4 Son polietilenoksit içeren bir üç bloklu kopolimer ise şu anda klinik denemeler geçiren kanser tedavisi. Klinik çalışmalarda misellerin 4 Four için beş polimerik misel formülasyonları PEG-bazlı çift bloklu kopolimerleri bulunması halinde. Bu misellerin büyüklüğü 20 nm ila 85 nm için değiştirilebilir. PEG bazlı polimerlerin kullanılmasının avantajı, bunların biyolojik uyumluluk ve ikinci blokta bağlı olarak biyo-bozunabilir de olabilir. Polietilenglikol blok -polylactic asit (-PLA b PEG), polimerik miseller göre en son yeni ilaç verme sistemleri birden fazla anti-kanser ilaçları eş zamanlı verilmesi için geliştirilmiştir. PEG-PLA b- misellerin bir biyouyumlu ve biyobozunur her ikisi de. Yüklenen miseller olarak göstermiştir bu çoklu ilaçynergistic vitro ve in vivo 2,5,6 farklı kanser modelleri önlenmesi ve direncini önleme kemoterapide birden fazla ilaç kullanan ve toksisiteyi düşürmek mevcut paradigma uyum sağlar. Bu nedenle, hazırlanması ve kanser ve diğer hastalık durumlarında kullanılmak üzere bu misel ilaç taşıyıcı sistemleri karakterize bir ilgi çok şey var. Çalışmada bu tür misel hazırlanmış ve ilgi hastalık durumlarında onları değerlendirilmeden önce karakterize edilebilir bir adım-adım süreci ana hatlarıyla aşağıda. Bu çalışmanın amacı için iki zayıf çözünen anti-kanser ajanları, dosetaksel (DTX) ve everolimus (EVR) seçilmiştir. DTX ve EVR Hem sırasıyla ml / 1.9 ve 9.6 ug içsel su çözünürlük ile suda az çözünen bileşiklerdir. Farklı moleküler ağırlıklara sahip 7,8 İki PEG b -PLA polimerler formüle polimer yapı taşları olarak bu protokolü kullanılmıştır miseller,-PLA 1800 (3800 Da) ve PEG 4000 b - - -PLA 2200 (6200 Da) b bu polimerler PEG 2000 bulunmaktadır. PEG-b -PLA miseller, bu nedenle DTX ve EVR tek tek ve kombinasyon halinde bir nanocarrier olarak benzersiz bir platform sağlar. Gerekli Reaktifler / Malzeme ve Ekipmanları hazırlamak ve bu misel Tablo 1&#39;de belirtilmiştir karakterize gerekiyordu.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>PEG2000-b-PLA1800</td>
			<td>Advanced Polymer Materials, Inc</td>
			<td>6-01- PLA/2000</td>
			<td>PLA MW can be specified on ordering</td>
		</tr>
		<tr>
			<td>PEG4000-b-PLA2200</td>
			<td>Advanced Polymer Materials, Inc</td>
			<td>6-01- PLA/4000</td>
			<td>PLA MW can be specified on ordering</td>
		</tr>
		<tr>
			<td>Docetaxel</td>
			<td>LC Laboratories</td>
			<td>D-1000</td>
			<td>100 mg</td>
		</tr>
		<tr>
			<td>Everolimus</td>
			<td>LC Laboratories</td>
			<td>E-4040</td>
			<td>100 mg</td>
		</tr>
		<tr>
			<td>Acetonitrile</td>
			<td>EMD/VWR</td>
			<td>EM-AX0145-1</td>
			<td>HPLC grade; 4 L</td>
		</tr>
		<tr>
			<td>Round bottom flask&#160;</td>
			<td>Glassco/VWR</td>
			<td>89426-496</td>
			<td>5 mL</td>
		</tr>
		<tr>
			<td>RV 10 Control Rotary Evaporators</td>
			<td>IKA Works</td>
			<td>8025001</td>
			<td>Rotoevaporator</td>
		</tr>
		<tr>
			<td>Shimadzhu HPLC with DAD detector</td>
			<td>Shimadzhu</td>
			<td></td>
			<td>RP-HPLC</td>
		</tr>
		<tr>
			<td>Slide-a-lyzer dialysis casette MWCO 7000</td>
			<td>Thermo Scientific, Inc</td>
			<td>66370</td>
			<td>3 mL</td>
		</tr>
		<tr>
			<td>Phosphate buffer pH 7.4 200 mM</td>
			<td>VWR</td>
			<td>100190-870</td>
			<td>500 mL</td>
		</tr>
		<tr>
			<td>Malvern NanoZS</td>
			<td>Malvern Instruments, UK</td>
			<td></td>
			<td>DLS</td>
		</tr>
		<tr>
			<td>Nylon filter</td>
			<td>Acrodisc/VWR</td>
			<td>28143-242</td>
			<td>13 mm; 0.2&#181;M</td>
		</tr>
		<tr>
			<td>Phosphoric acid, NF</td>
			<td>Spectrum Chemical/VWR</td>
			<td>700000-626</td>
			<td>100 mL</td>
		</tr>
		<tr>
			<td>GraphPad Prism</td>
			<td><a href="http://www.graphpad.com/">www.graphpad.com</a></td>
			<td></td>
			<td>Analysis software</td>
		</tr>
		<tr>
			<td>Zorbax SB-C8 Rapid Resolution cartridge&#160;</td>
			<td>Agilent Technologies</td>
			<td>866953-906</td>
			<td>4.6 &#215;75mm, 3.5 micron</td>
		</tr>
	</tbody>
</table>

preparation and characterization of individual and multi-drug loaded physically entrapped polymeric micelles

Polietilenglikol blok -polylactic asit (PLA b- PEG) gibi bir amfifilik blok kopolimerleri, sulu ortamlarda hidrofilik kabuğuyla çevrelenmiş hidrofobik çekirdekler oluşturulmasını kritik misel konsantrasyonunun üzerinde miseller halinde kendi kendine birleşebilen olabilir. Bu misellerin çekirdek dosetaksel (DTX) ve everolimus (EVR) gibi hidrofobik, suda çözünürlüğü zayıf olan ilaçların yüklemek için kullanılabilir. Misel yapısı ve ilaç yükleme özellikleri sistematik karakterizasyonu yapılabilir in vitro ve in vivo çalışmalar önce önemlidir. Bu tarifnamede tarif edilen protokol amacı standart misel ürünler elde etmek için gerekli olan karakterizasyon adımları sağlamaktır. DTX ve EVR, sırasıyla, bu misellerin hazırlanışı, sırasıyla 1.86 ve 1.85 mg / ml için DTX ve EVR suda çözünürlüğünü arttırır solvent döküm yoluyla elde edilebilir ml / 1.9 ve 9.6 ug içsel çözünürlüklere sahiptir. Eval miseller ilaç stabilitesi48 saat boyunca oda sıcaklığında değerlendirmeler yapılmıştır ilaçların% 97 ya da daha fazla çözelti içinde muhafaza ettiğini göstermektedir. Misel boyutu, dinamik ışık saçılması ile değerlendirildi ve bu misellerin büyüklüğü 50 nm&#39;nin altında ve polimerin molekül ağırlığına bağlı olduğu belirtilmiştir. Misellerin gelen ilaç salım 48 saat içinde 37 o C&#39;de pH 7.4&#39;te lavabo koşullarında diyaliz kullanılarak değerlendirildi. Eğri uydurma sonuçlar ilaç salım difüzyon tahrik belirten birinci dereceden bir işlem tarafından tahrik edilir olduğunu göstermektedir.

Bireysel DTX veya EVR miselleri ve miseller başarıyla PEG 4000 ya formüle edilir -PLA b PEG içinde DTX ve EVR DDM - b -PLA 2200 veya PEG 2000 - b -PLA 1800 (Şekil 1). DTX EVR ve DDM PEG 4000 içindeki kararlılık göstermiştir - 48 saatten fazla bir -PLA 1800 b (Şekil 2) - -PLA 2200 veya PEG 2000, b. -PLA 2200,...

Watch this Scientific Journal Video about Preparation and Characterization of Individual and Multi-drug Loaded Physically Entrapped Polymeric Micelles at JoVE.com

Preparation and Characterization of Individual and Multi-drug Loaded Physically Entrapped Polymeric Micelles

The goal of this protocol is to describe the preparation and characterization of physically entrapped, poorly water soluble drugs in micellar drug delivery systems composed of amphiphilic block copolymers.

Hazırlanması ve Bireysel Karakterizasyonu ve Multi-ilaç Fiziksel, polimerik misellerin Entrapped Loaded

Amphiphilic block copolymers like polyethyleneglycol-block-polylactic acid (PEG-b-PLA) can self-assemble into micelles above their critical micellar ...

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11.2K Görüntüleme.  Pacific University. The goal of this protocol is to describe the preparation and characterization of physically entrapped, poorly water soluble drugs in micellar drug delivery systems composed of amphiphilic block copolymers.

Video: Preparation and Characterization of Individual and Multi-drug Loaded Physically Entrapped Polymeric Micelles

Split-and-pool Synthesis and Characterization of Peptide Tertiary Amide Library

Peptidomimetics are great sources of protein ligands. The oligomeric nature of these compounds enables us to access large synthetic libraries on solid phase by using combinatorial chemistry. One of the most well studied classes of peptidomimetics is peptoids. Peptoids are easy to synthesize and have been shown to be proteolysis-resistant and cell-permeable. Over the past decade, many useful protein ligands have been identified through screening of peptoid libraries. However, most of the ligands identified from peptoid libraries do not display high affinity, with rare exceptions. This may be due, in part, to the lack of chiral centers and conformational constraints in peptoid molecules. Recently, we described a new synthetic route to access peptide tertiary amides (PTAs). PTAs are a superfamily of peptidomimetics that include but are not limited to peptides, peptoids and N-methylated peptides. With side chains on both &#945;-carbon and main chain nitrogen atoms, the conformation of these molecules are greatly constrained by sterical hindrance and allylic 1,3 strain. (Figure 1) Our study suggests that these PTA molecules are highly structured in solution and can be used to identify protein ligands. We believe that these molecules can be a future source of high-affinity protein ligands. Here we describe the synthetic method combining the power of both split-and-pool and sub-monomer strategies to synthesize a sample one-bead one-compound (OBOC) library of PTAs.

Peptide tertiary amides (PTAs) are a superfamily of peptidomimetics that include but are not limited to peptides, peptoids and N-methylated peptides. Here we describe a synthetic method which combines&#160;both split-and-pool and sub-monomer strategies to synthesize a one-bead one-compound library of PTAs.

Split-ve-havuz Sentezi ve Peptit Tersiyer Amid Kütüphanesi Karakterizasyonu

Peptidomimetics are great sources of protein ligands. The oligomeric nature of these compounds enables us to access large synthetic libraries on solid ...

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 ...

Preparation and Characterization of SDF-1&#945;-Chitosan-Dextran Sulfate Nanoparticles

Chitosan (CS) and dextran sulfate (DS) are charged polysaccharides (glycans), which form polyelectrolyte complex-based nanoparticles when mixed under appropriate conditions. The glycan nanoparticles are useful carriers for protein factors, which facilitate the in vivo delivery of the proteins and sustain their retention in the targeted tissue. The glycan polyelectrolyte complexes are also ideal for protein delivery, as the incorporation is carried out in aqueous solution, which reduces the likelihood of inactivation of the proteins. Proteins with a heparin-binding site adhere to dextran sulfate readily, and are, in turn, stabilized by the binding. These particles are also less inflammatory and toxic when delivered in vivo. In the protocol described below, SDF-1&#945; (Stromal cell-derived factor-1&#945;), a stem cell homing factor, is first mixed and incubated with dextran sulfate. Chitosan is added to the mixture to form polyelectrolyte complexes, followed by zinc sulfate to stabilize the complexes with zinc bridges. The resultant SDF-1&#945;-DS-CS particles are measured for size (diameter) and surface charge (zeta potential). The amount of the incorporated SDF-1&#945; is determined, followed by measurements of its in vitro release rate and its chemotactic activity in a particle-bound form.

Preparation and Characterization of SDF-1&amp;#945;-Chitosan-Dextran Sulfate Nanoparticles

The objective of this protocol is to incorporate SDF-1&#945;, a stem cell homing factor, into dextran sulfate-chitosan nanoparticles. The resultant particles are measured for their size and zeta potential, as well as the content, activity, and in vitro release rate of SDF-1&#945; from the nanoparticles.

SDF-1α-Kitosan-Dekstran Sülfat nano partiküllerin hazırlanması ve Karakterizasyonu

Chitosan (CS) and dextran sulfate (DS) are charged polysaccharides (glycans), which form polyelectrolyte complex-based nanoparticles when mixed under ...

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 ...

Low-energy Cathodoluminescence for (Oxy)Nitride Phosphors

Nitride and oxynitride (Sialon) phosphors are good candidates for the ultraviolet and visible emission applications. High performance, good stability and flexibility of their emission properties can be achieved by controlling their composition and dopants. However, a lot of work is still required to improve their properties and to reduce the production cost. A possible approach is to correlate the luminescence properties of the Sialon particles with their local structural and chemical environment in order to optimize their growth parameters and find novel phosphors. For such a purpose, the low-voltage cathodoluminescence (CL) microscopy is a powerful technique. The use of electron as an excitation source allows detecting most of the luminescence centers, revealing their luminescence distribution spatially and in depth, directly comparing CL results with the other electron-based techniques, and investigating the stability of their luminescence properties under stress. Such advantages for phosphors characterization will be highlighted through examples of investigation on several Sialon phosphors by low-energy CL.

Low-energy Cathodoluminescence for OxyNitride Phosphors

An excellent chemical and luminescence stabilities of (oxy)nitride phosphors present it as an promising alternative to currently used sulfide and oxide phosphors. In this paper, we present the way to investigate its local luminescence properties using low-energy cathodoluminescence (CL).

(Oxy) Nitrit Fosforilazın için düşük enerji Katodolüminesans

Nitride and oxynitride (Sialon) phosphors are good candidates for the ultraviolet and visible emission applications. High performance, good stability and ...

Facile Synthesis of Worm-like Micelles by Visible Light Mediated Dispersion Polymerization Using Photoredox Catalyst

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins with the synthesis of a hydrophilic poly(oligo(ethylene glycol) methyl ether methacrylate) (POEGMA) homopolymer using reversible addition-fragmentation chain-transfer (RAFT) polymerization. Under mild visible light irradiation (&#955; = 460 nm, 0.7 mW/cm2), this macro-chain transfer agent (macro-CTA) in the presence of a ruthenium based photoredox catalyst, Ru(bpy)3Cl2 can be chain extended with a second monomer to form a well-defined block copolymer in a process known as Photoinduced Electron Transfer RAFT (PET-RAFT). When PET-RAFT is used to chain extend POEGMA with benzyl methacrylate (BzMA) in ethanol (EtOH), polymeric nanoparticles with different morphologies are formed in situ according to a polymerization-induced self-assembly (PISA) mechanism. Self-assembly into nanoparticles presenting POEGMA chains at the corona and poly(benzyl methacrylate) (PBzMA) chains in the core occurs in situ due to the growing insolubility of the PBzMA block in ethanol. Interestingly, the formation of highly pure worm-like micelles can be readily monitored by observing the onset of a highly viscous gel in situ due to nanoparticle entanglements occurring during the polymerization. This process thereby allows for a more reproducible synthesis of worm-like micelles simply by monitoring the solution viscosity during the course of the polymerization. In addition, the light stimulus can be intermittently applied in an ON/OFF manner demonstrating temporal control over the nanoparticle morphology.

This article describes a process for producing polymeric self-assembled nanoparticles using visible light mediated dispersion polymerization. Using low energy visible light to control the polymerization allows for the reproducible formation of self-assembled worm-like micelles at high solids content.

Photoredox Katalizörü kullanarak görünür ışık aracılığı ile dispersiyon polimerleştirilmesi ile solucan gibi miseller Facile sentezi

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins ...

Anionic Polymerization of an Amphiphilic Copolymer for Preparation of Block Copolymer Micelles Stabilized by &#960;-&#960; Stacking Interactions

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE). Characterization of the copolymer revealed a narrow molecular distribution (PDI &#60; 1.03) and confirmed the degree of polymerization of mPEG122-b-(PheGE)15. The critical micelle concentration of the copolymer was evaluated using an established fluorescence method with the aggregation behavior evaluated by dynamic light scattering and transmission electronic microscopy. The potential of the copolymer for use in drug delivery applications was evaluated in a preliminary manner including in vitro biocompatibility, loading and release of the hydrophobic anti-cancer drug doxorubicin (DOX). A stable micelle formulation of DOX was prepared with drug loading levels up to 14% (wt%), drug loading efficiencies &#62; 60% (w/w) and sustained release of drug over 4 days under physiologically relevant conditions (acidic and neutral pH, presence of albumin). The high drug loading level and sustained release is attributed to stabilizing &#960;-&#960; interactions between DOX and the core-forming block of the micelles.

Anionic Polymerization of an Amphiphilic Copolymer for Preparation of Block Copolymer Micelles Stabilized by &amp;#960;-&amp;#960; Stacking Interactions

The key steps of living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE) are described. The resulting block copolymer micelles (BCMs) were loaded with doxorubicin 14% (wt%) and sustained release of drug over 4 days under physiologically relevant conditions was obtained.

π-π İstifleme etkileşimlerle Stabilize blok kopolimer miselleri hazırlanması için bir amfifilik kopolimerin anyonik polimerizasyonu

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl ...

Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single molecule level. An electrostatic self-assembly and covalent fixation (ESA-CF) process is used for the synthesis of the cyclic poly(tetrahydrofuran) (poly(THF)). The diffusive motion of individual cyclic polymer chains in a melt state is visualized using single molecule fluorescence imaging by incorporating a fluorophore unit in the cyclic chains. The diffusive motion of the chains is quantitatively characterized by means of a combination of mean-squared displacement (MSD) analysis and a cumulative distribution function (CDF) analysis. The cyclic polymer exhibits multiple-mode diffusion which is distinct from its linear counterpart. The results demonstrate that the diffusional heterogeneity of polymers that is often hidden behind ensemble averaging can be revealed by the efficient synthesis of the cyclic polymers using the ESA-CF process and the quantitative analysis of the diffusive motion at the single molecule level using the MSD and CDF analyses.

A protocol for the synthesis and characterization of diffusive motion of cyclic polymers at the single molecule level is presented.

Tek Molekül Düzeyde Halkalı Polimerlerin Sentezi ve eritin Devlet Onların Pasif Hareket Karakterizasyonu

We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single ...

Synthesis of Plant Phenol-derived Polymeric Dyes for Direct or Mordant-based Hair Dyeing

Effective hair dyeing through in situ incubation of keratin hair with the products of fungal laccase-catalyzed polymerization of plant phenols has been previously demonstrated. However, the dyeing process takes a long time to complete compared to commercial hair-dyeing products. To overcome this bottleneck, pre-synthesized polymeric products of the oxidative reaction of Trametes versicolor laccase on catechin and catechol, either with or without mordant agents (e.g., FeSO4), were here employed to achieve permanent keratin hair dyeing in various colors and shades. The laccase action in acidic sodium acetate buffer led to a deep black coloration after coupling reactions between the plant phenols. The colored dye products were then desalted and concentrated with ultrafiltration. The dyes, with or without mordant agents, caused a significant increase in &#916;E values (i.e., color difference value) in gray human hair within 2.5 hours. In addition, different keratin colors and shades were induced depending upon the mordanting and pH changes. The dyed hair also exhibited a strong resistance to detergent treatments, indicating that our methods can give rise to permanent hair dyeing.&#160;Overall, our work has provided novel insight into developing eco-friendly hair-dyeing methods as alternatives to commercial toxic diamine-based dyes.

Here, we present a protocol to use pre-synthesized polymeric products derived from fungal laccase-catalyzed polymerization of plant phenols, either with or without mordant agents (e.g., FeSO4), to induce detergent-resistant keratin hair dyeing within 2.5 hours.

Doğrudan ya da Mordan tabanlı Saç Boyama için Bitki Fenol türevli Polimerik Boyaların Sentezi

Effective hair dyeing through in situ incubation of keratin hair with the products of fungal laccase-catalyzed polymerization of plant phenols has been ...

Preparation and In Vitro Characterization of Dendrimer-based Contrast Agents for Magnetic Resonance Imaging

Paramagnetic complexes of gadolinium(III) with acyclic or macrocyclic chelates are the most commonly used contrast agents (CAs) for magnetic resonance imaging (MRI). Their purpose is to enhance the relaxation rate of water protons in tissue, thus increasing the MR image contrast and the specificity of the MRI measurements. Current clinically approved contrast agents are low molecular weight molecules that are rapidly cleared from the body. The use of dendrimers as carriers of paramagnetic chelators can play an important role in the future development of more efficient MRI contrast agents. Specifically, the increase in local concentration of the paramagnetic species results in a higher signal contrast. Furthermore, this CA provides a longer tissue retention time due to its high molecular weight and size. Here, we demonstrate a convenient procedure for the preparation of macromolecular MRI contrast agents based on poly(amidoamine) (PAMAM) dendrimers with monomacrocyclic DOTA-type chelators (DOTA &#8211; 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate). The chelating unit was appended by exploiting the reactivity of the isothiocyanate (NCS) group towards the amine surface groups of the PAMAM dendrimer to form thiourea bridges. Dendrimeric products were purified and analyzed by means of nuclear magnetic resonance spectroscopy, mass spectrometry, and elemental analysis. Finally, high resolution MR images were recorded and the signal contrasts obtained from the prepared dendrimeric and the commercially available monomeric agents were compared.

Preparation and In Vitro Characterization of Dendrimer-based Contrast Agents for Magnetic Resonance Imaging

This protocol describes the preparation and characterization of a dendrimeric magnetic resonance imaging (MRI) contrast agent that carries cyclen-based macrocyclic chelates coordinating paramagnetic gadolinium ions. In a series of MRI experiments in vitro, this agent produced an amplified MRI signal when compared to the commercially available monomeric analogue.

Hazırlama ve<em&gt; İn Vitro</em&gt; Manyetik Rezonans Görüntüleme için Dendrimer tabanlı Kontrast Ajanlar Karakterizasyonu

Paramagnetic complexes of gadolinium(III) with acyclic or macrocyclic chelates are the most commonly used contrast agents (CAs) for magnetic resonance ...