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.

참고 : 시작하기 전에, 모든 관련 자료 데이터 시트 (MSDS (물질 안전 보건 자료))을 확인. 합성 절차 및 애플리케이션에 사용되는 화학 물질 중 일부는 독성. 모든 적절한 안전 관행에 따라 적절한 보호 장비 (실험실 코트, 전체 길이 바지, 폐쇄 발가락 신발, 보호 안경, 장갑)를 사용하십시오. 질소 흡착 측정을위한 액체 질소 (절연 장갑, 얼굴 가리개)를 처리 할 때 모든 극저온 개인 보호 장비를 사용하십시오. 벌크 및 모세관 컬럼 형식의 1 다공성 고분자 모노리스 준비 <ol><li> 특성에 대한 대량 폴리머 모노리스 <ol><li> 중합 억제제를 제거하기 위해, 염기성 알루미나 컬럼을 통해 스티렌, 디 비닐 벤젠 및 메타 크릴 산을 정제. 주사기 팁에 포장 유리 양모 섬유의 플러그가있는 25 ml의 일회용 플라스틱 주사기에 기본 알루미나 10g을 놓습니다. 칼럼을 통해 단량체의 약 10 ㎖을 관류. </li><li> 단량체 (50 mg의 스티렌, 디 비닐 벤젠 100 mg을 50 mg의 메타 크릴 산) 및 1 mL 유리 바이알에 기공 형성 제 (300 mg을 톨루엔 및 300 mg을 이소옥탄)을로드. 중합 개시제 2,2&#39;- 아조 비스 이소 부티로 니트릴 (AIBN, 단량체에 대하여 1 %) 4 mg을 추가. </li><li> 10 분 동안 초음파 처리하여 균질화. 10 분 동안 액체를 통해 질소를 버블 링하여 용존 산소를 제거합니다. 파라핀 필름으로 유리 병 마개를 밀봉하고, 혼합물을 중합하기 위해 6 시간 동안 60 ℃에서 수조에 배치. </li><li> 실온으로 냉각 조심스럽게 병을 깰. 셀룰로오스 추출 골무에 폴리머 기둥을 전송합니다. 속 슬렛 추출 챔버로 추출 골무를 놓고 추출 챔버의 적어도 세 번 볼륨 메탄올의 부피를 포함하는 둥근 바닥 플라스크를 조립한다. 추출 챔버의 상부에 콘덴서를 조립한다. 메탄올을 끓여 속 슬렛 추출을 수행16 시간 동안, 미 반응 단량체의 완전한 제거를 보장하고 기공 형성 제. </li><li> 60 ℃에서 진공 오븐에서 하룻밤 동안 건조. 푸리에에 의해 주치의 적외선 분광법 (FT-IR)를 변환 첨부 카르 복실 작용기의 존재를 확인합니다. 질소 흡착 세공 측정법에 의해 비 표면적을 측정한다. </li></ol></li><li> 모 놀리 식 기둥의 준비를 위해 실리카 모세 혈관의 작용 <ol><li> 폴리이 미드 코팅 된 100 ㎛의 ID 용융 실리카 모세관의 2m를 잘라. 0.25-0.50 mL 유리 주사기에 연결하고 아세톤으로 모세관을 씻는다. 물과 모세 혈관을 세척하여 아세톤을 제거합니다. </li><li> 모세관 내부의 실리카 코팅을 활성화하기 위해, 30 분 / μL에서 0.25 분, 0.2 M 수성 NaOH 용액을 흐르게 주사기 펌프를 사용한다. 유출 물이 중성이 될 때까지 물로 씻어. </li><li> 폐수의 pH를 확인 산도 종이 스트립을 사용합니다. 모세관의 실란 올 그룹을 양성자 화하기 위해, 0.2 M aqueo 펌프30 분 동안 0.25 μL / 분 모세관을 통해 우리 HCl 용액. 유출 물이 중성이 될 때까지 물로 씻어. 에탄올로 씻어. </li><li> 1 시간 / μL로 0.25 분 (w / w) 20 % 3- (트리 메 톡시 실릴) 프로필 메타 크릴 레이트 (아세트산으로 pH를 조정 5)의 에탄올 용액 펌프. 이 단계에서, 실리카 모세관은 모세관 내면 중합체 모노리스를 장착하기 위해 비닐기로 작용 화한다. </li><li> 질소 기류, 아세톤으로 세척하여 건조 밤새 사용하기 전에 실온에서 떠난다. 길이 20cm의 짧은 조각으로 모세관을 잘라. </li></ol></li><li> 모 놀리 식 모세관 컬럼의 준비 <ol><li> 고무 격막과 1 mL 유리 병에 일괄 폴리머 모노리스 (1.1 절)에 대해서는 동일한 중합 혼합물을 준비합니다. 단량체에 대해 기자에게 1 %의 AIBN을 추가합니다. 10 분 동안 초음파 처리하여 균질화. </li><li> 비 - 관능 화 실리카 모세관을 커플 링시킴으로써 질소로 중합 혼합물 퍼지질소 스트림. <ol><li> 유리 병의 고무 격막을 통해 질소 기류 모세관을 삽입하고 질소는 액체를 통해 거품 있도록 중합 혼합물로 몰입. 과도한 압력을 피하기 위해 약간 느슨한 유리 병 뚜껑을 남겨주세요. 10 분 동안 퍼징. </li><li> 바이알의 헤드 스페이스에 중합 혼합물로부터 질소 기류 모세관을 들어 올리고 뚜껑을 꼭 닫습니다. 중합 혼합물에 격막을 통해 작용 모세관을 삽입합니다. 상부 공간에 주입 된 질소를 통해 모세관에 생성 된 압력의 초과는 모세관 작용을 통해 중합 반응 혼합물을 펌프. </li><li> 완전히 충전되어 있는지 확인하고 고무 격막을 닫습니다 모세관의 유출에서 중합 혼합물의 몇 방울을 수집합니다. 매우 신중하게 유리 병 밖으로 모세관을 가지고 고무 격막에 모세관의 입구를 닫습니다. </li></ol></li><li> 믹스를 중합6 시간 동안 60 ℃에서 수욕 모세관에 포함 스트럭처. 실온에서 냉각시키고, 모세관 양단의 몇 밀리미터를 잘랐다. 30 분 동안 3 μL / min으로 HPLC 펌프를 사용하여 아세토 니트릴로 열을 세척하여 미 반응 모노머 및 기공 형성 제를 제거합니다. 모세관 컬럼의 배압을 확인합니다. </li></ol></li></ol> 철 benzenetrycarboxylate 2. 성장 (FeBTC) PCP <ol><li> 특성에 대한 대량 폴리머 모노리스에 FeBTC MOPH의 성장 <ol><li> 박격포와 유 봉을 사용하여 이전에 건조 된 모노리스를 갈기. </li><li> 15 분 동안 2 mM의 에탄올의 FeCl3 · 6H 2 O 5 ml의 모노리스 분말 100mg을 담가. 나일론 필터 (0.22 μm의)와 에탄올로 가루를 씻어을 사용하여 진공 필터. 15 분 동안 에탄올에서 2 mM의 1,3,5- 벤젠 트리 카르 복실 산 (BTC) 5ml에 모노리스 분말을 담근다. 나일론 필터 (0.22 μm의)와 에탄올로 가루를 씻어을 사용하여 진공 필터.</li><li> 원하는대로 단계를 반복 번호 2. 최종 금속 - 유기 피막의 성장이 적용 사이클의 수에 의해 정의 될 뿐이다. 일반적으로 10 ~ 30 사이클이 수행됩니다. 질소 흡착 압 입법에 의한 새로운 구멍의 존재를 확인합니다. 열 중량 분석 (TGA)에 의해 추가 된 금속 부위의 양을 측정한다. </li></ol></li><li> 포스 포의 농축을위한 모세관 모 놀리 식 열에 FeBTC MOPH의 성장 <ol><li> 주사기 펌프를 이용. 2 μL / 분으로 15 분 동안 2 mM의 에탄올 중의 FeCl3 · 6H 2 O와 모세관 모노리스 플러시. 2 μL / 분에서 15 분 동안 에탄올로 씻으십시오. 2 μL / 분에서 15 분간 에탄올에서 2 mM의 BTC와 모세관 모노리스 플러시. 2 μL / 분에서 15 분 동안 에탄올로 씻으십시오. </li><li> 필요에 따라 1 단계를 반복합니다. 최종 금속 - 유기 피막의 성장이 수행 사이클의 수에 의해 정의 될 뿐이다. </li></ol></li></ol> 3. 단백질 소화와 E포스 포의 nrichment <ol><li> 단백질 소화 <ol><li> 물 1 ㎖에 무 지방 우유 0.5 ㎖에 용해시키고, 200 μL 분획으로 나눈다. </li><li> 단백질 소화 이황화 결합을 절단하기 위해, 각각의 분획을 160 ㎕의 1 M 중탄산 암모늄 및 50 ㎕의 45 mM의 디티 오 트레이 톨을 추가한다. 15 분 동안 써모에서 50 ° C에서 인큐베이션. </li><li> 용액 내려 실온으로 냉각하면서, 요오도 아세트 아미드 100 mM이 수용액 서서히 50 μl를 추가. 요오도 아세트 아미드는 새로운 이황화 결합의 형성을 방지한다. </li><li> 실온에서 15 분 동안 어두운 데에서 인큐베이션. 탈 이온수 1 ML을 추가합니다. 14 시간 동안 37 ℃에서 써모에서 단백질을 2 μg의 트립신을 추가하고 소화. </li><li> 1 % 트리 플루오로 아세트산 10 μL로 산성화하여 소화를 종료하고, 실온에서 5 분 동안 써모에 배치. 소화 단백질에 보관 -20 ° C. </li></ol></li><li> 모세관 MOPH 열을 사용하는 포스 포의 농축. <ol><li> 1 μL / 분의 유속에서 10 분 동안 0.1 % 트리 플루오로 아세트산 함유 아세토 니트릴의 1 : 1 혼합물 100 ㎕ 4와 칼럼 플러시. 30 분 / 2 μL에서 분 칼럼을 통해 단백질 소화 펌프. </li><li> 1 μL / 분의 유속에서 10 분 동안 0.1 % 트리 플루오로 아세트산 함유 아세토 니트릴의 혼합물을 1 : 4로 다시 인산화되지 않은 펩티드를 세척 할 것. 1 μL / 분의 유속으로 10 분 동안 물로 세척한다. </li><li> 15 분 동안 1 μL / 분으로 펌핑 된 250 mM의 pH가 7 인산염 완충액을 사용하여 용출 포스 포. 유리 병에 용리액을 수집하고 표준 프로토콜 19을 사용하여 솔루션을 탈염. 매트릭스 보조 레이저 탈착 / 이온화 비행 시간 형 질량 분석계 (MALDI-TOF-MS)에 대한 매트릭스로서 사용하는 2 ㎎ / ㎖ 2,5- 디 히드 록시 벤조산을 준비한다. phosphope을 용출하는 팁에 2,5- 디 히드 록시 벤조산의 2 μl를 그린ptides는 MALDI 판에 직접 자리합니다. </li><li> MALDI-TOF-MS에 의해 명소를 분석하고 물과 메탄올로 충분히 세척하여 열을 생성합니다. </li></ol></li></ol>

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A. 1217, 902-924 (2010).</li><li>Shekhah, O., 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=Step-by-step+route+for+the+synthesis+of+metal-organic+frameworks.">Step-by-step route for the synthesis of metal-organic frameworks.</a> J. Am. Chem. Soc. 129, 15118-15119 (2007).</li><li>Shekhah, O., Fu, L., Belmabkhout, Y., Cairns, A. J., Giannelis, E. P., Eddaoudi, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Successful+implementation+of+the+stepwise+layer-by-layer+growth+of+MOF+thin+films+on+confined+surfaces:+mesoporous+silica+foam+as+a+first+case+study.">Successful implementation of the stepwise layer-by-layer growth of MOF thin films on confined surfaces: mesoporous silica foam as a first case study.</a> Chem. Commun. 48, 11434-11436 (2012).</li><li>Saeed, A., Maya, F., Xiao, D. J., Naham-ul-Haq, M., Svec, F., Britt, D. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Growth+of+a+highly+porous+coordination+polymer+on+a+macroporous+polymer+monolith+support+for+enhanced+immobilized+metal+ion+affinity+chromatographic+enrichment+of+phosphopeptides.">Growth of a highly porous coordination polymer on a macroporous polymer monolith support for enhanced immobilized metal ion affinity chromatographic enrichment of phosphopeptides.</a> Adv. Funct. Mater. 24, 5797-5710 (2014).</li><li>Krenkova, J., Lacher, N. 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Chem. 84, 10180-10185 (2012).</li><li>Hussain, D., 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=Functionalized+diamond+nanopowder+for+phosphopeptides+enrichment+from+complex+biological+fluids.">Functionalized diamond nanopowder for phosphopeptides enrichment from complex biological fluids.</a> Anal. Chim. Acta. 775, 75-84 (2013).</li><li>Aprilita, N. H., 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=Poly(glycidyl+methacrylate/divinylbenzene)-IDA-FeIII+in+phosphoproteomics.">Poly(glycidyl methacrylate/divinylbenzene)-IDA-FeIII in phosphoproteomics.</a> J. Proteom. Res. 4, 2312-2319 (2005).</li><li>Lo, C. Y., Chen, W. Y., Chen, C. T., Chen, Y. 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The authors have nothing to disclose.

원래 고분자 모노리스는 금속에 결합 할 수 카르 복실 작용기를 포함하고 있습니다. 원래 소재에 초기 금속 자리 코디 우리 미다 네트워크 정형 추가적인 금속 자리의 숫자를 통합 PCP 코팅 (도 1a)을 성장할 수있다. 이것은 고정 된 금속 이온 친 화성 크로마토 그래피 (IMAC) 기술과 같은 금속의 종 관련된 추출 또는 정제 과정, 매력적인 제시된 MOPH 재료를 만든다. 포스 포의 농축 용 캐 ?...

다공성 배위 고분자 (의 PCP)는 비정질 또는 결정질 일 수있다 1-3 1, 2 또는 3 차원으로 연장되는 조정 엔티티 반복 유기 리간드에 의해 연결된 금속 중심에 기초한 배위 화합물이다. 최근에, 다공성 물질이 클래스는 그들의 높은 다공성, 넓은 화학 가변성, 및 안정성으로 널리 주목 받고있다. 의 PCP는 가스 저장, 가스 분리 및 촉매 3-6, 매우 최근의 PCP의 분석 애플리케이션 제 7 기술되었다을 포함한 다양한 애플리케이션에 대해 탐구되어왔다. 때문에 강화 화학 기능과 높은 기공율의 PCP 정제 공정 및 크로마토 그래피 분리의 개선을위한 그들의 엄청난 잠재적 대상으로되어 있고,이 항목에 관한 다수의 보고서가 7-13 발표되었다. 그러나,의 PCP의 성능 equivale에서 현재 사용하지 않는그들의 입자 또는 결정의 그들의 일반적으로 불규칙한 모양의 형태학에 의한 이러한 고체의 충전 층에서 큰 입자 간 공극을 통해 빠르게 확산 가능성이 기존의 크로마토 그래피 재료와 NT 수준. 이 불규칙하게 분산 포장 낮은 예상보다 성능뿐만 아니라 높은 열 배압 및 바람직하지 않은 피크 모양 형태학 14, 15로 연결됩니다. 입자 간 공극을 통해 빠르게 확산의 문제를 해결하고 부수적 분석 애플리케이션의 PCP의 성능을 향상시키기 위하여, 거대 기공의 표면에 PCP를 포함하는 거대 다공성 중합체 모노리스 (16)에 기초하여 복합 재료의 개발하고자 것이 바람직하다. 고분자 모노리스 패킹 비드 성공적 여러 C 상용화되어 가장 효율적인 대안들 중 하나를들을 수있는, 그들의 구멍을 통해 대류 흐름을 유지할 수 단일 피스 재료 자체 포함 된<html> ompanies (17, 18). 다공성 중합체는 일반적으로 모노리스 단량체의 중합, 전형적으로 유기 용매의 혼합물이다 이진 포로 겐의 존재 하에서 가교제에 기초한다. 얻어진 재료는 모 놀리 microglobular 구조 및 높은 다공성 및 유동 투과도. 간단한 방법은 PCP를 함유하는 중합체 단일체 모노리스의 중합 혼합물의 PCP 합성 된 상태의 직접 첨가에 기초 제조 이들 재료를 통합한다. 결과의 PCP이 방식은 주로 최종 14,15 재료의 상기 어플리케이션에 대해 활성 인 고분자 지지체 내에 매립되는 것은 아니다. 다른 합성 방법이 명확하게, 예를 들면, 결정에 포함 된 기공의 대부분이 중합체 모노리스의 거대에서 액세스의 PCP, 또는 결정 성 금속 - 유기 프레임 워크 (MOFs는)의​​ 균일 한 필름을 개발하기 위해 필요하다. t &quot;&gt; 여기서 우리는 쉽게 구현 될 수의 PCP의 부착에 적합한 작용기를 가진 거대 다공성 고분자 지지체에 기초한 유기 금속 중합체 복합 재료 (MOPH)의 제조를위한 간단한 프로토콜보고 급식 단일 관류 애플리케이션을위한 최적의 특성을 갖는 열 형식 -piece 중합체 모놀리스. 중합체 합성 절차가 간단 실온 용액 기반 뒤에 &#160; 방법 19-20 모노리스의 공극의 내부 표면 상에 코팅 PCP 성장. 첫 번째 예로서, 우리는 거대 다공성 폴리 (스티렌 - 디 비닐 벤젠 - 메타 크릴 산) 모노리스 내의 철 (III) 벤젠 (FeBTC) 배위 고분자 필름의 제조를 기술한다. 이 방법은 벌크 분말의 제조뿐만 아니라, 캐 필러 리 컬럼을위한 효과적이고 설명은 다른 프로토콜의 PCP에게 용이하게 구현 가능하다. 유동 throu위한 기능성 재료로서 MOPHs의 전위의 예로서GH 응용 프로그램, 우리는 센터가 철에 포스 포의 결합 친화력을 악용 소화 단백질 혼합물에서 포스 포 농축 (III) 철의 고밀도 코팅을 포함하는 개발 FeBTC MOPH을 적용 (III). 개발 된 프로토콜 (21)는 세 가지 주요 부분 : 상기 거대 다공성 유기 고분자 모노리스 지원 준비; 모노리스의 기공의 표면에 코팅 PCP의 성장; 포스 포의 농축을위한 응용 프로그램입니다.

<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.

유기 고분자 모노리스의 기공 표면에 PCP 성장의 개략도는도 1에 도시된다.이 도면에서, 우리는 예시 초기의 Fe (III) 원자 복실 작용기에 배위 원래 중합체 모노리스의 기공 표면에 보유 . 프로토콜을 사용하는 것은 본원에 추가로 유기 리간드와 설명의 Fe (III) 이온이 중합체 모노리스 내의 다공질 코디 네트워크를 성형 표면에 첨가된다. 또한 개략적위한 관류 지지체로서 준비한 모세?...

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

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.

포스 포의 향상된 농축을위한 거대 다공성 고분자 모노리스에 다공성 조정 폴리머 코팅의 제조

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

preparation-highly-porous-coordination-polymer-coatings-on

Research

JoVE Journal

Chemistry

10.0K 조회수.  E. O. Lawrence Berkeley National Laboratory. 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.

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

Confocal Imaging of Confined Quiescent and Flowing Colloid-polymer Mixtures

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed assembly1-3, drug delivery4, improved hydrocarbon recovery5-7, and flowable electrodes for energy storage8. Suspensions containing fluorescent colloids and non-adsorbing polymers are appealing model systems, as the ratio of the polymer radius of gyration to the particle radius&#160;and concentration of polymer control the range and strength of the interparticle attraction, respectively. By tuning the polymer properties and the volume fraction of the colloids, colloid fluids, fluids of clusters, gels, crystals, and glasses can be obtained9.&#160;Confocal microscopy, a variant of fluorescence microscopy, allows an optically transparent and fluorescent sample to be imaged with high spatial and temporal resolution in three dimensions. In this technique, a small pinhole or slit blocks the emitted fluorescent light from regions of the sample that are outside the focal volume of the microscope optical system. As a result, only a thin section of the sample in the focal plane is imaged. This technique is particularly well suited to probe the structure and dynamics in dense colloidal suspensions at the single-particle scale: the particles are large enough to be resolved using visible light and diffuse slowly enough to be captured at typical scan speeds of commercial confocal systems10. Improvements in scan speeds and analysis algorithms have also enabled quantitative confocal imaging of flowing suspensions11-16,37.&#160;In this paper, we demonstrate confocal microscopy experiments to probe the confined phase behavior and flow properties of colloid-polymer mixtures. We first prepare colloid-polymer mixtures that are density- and refractive-index matched. Next, we report a standard protocol for imaging quiescent dense colloid-polymer mixtures under varying confinement in thin wedge-shaped cells. Finally, we demonstrate a protocol for imaging colloid-polymer mixtures during microchannel flow.

Confocal microscopy is used to image quiescent and flowing colloid-polymer mixtures, which are studied as model systems for attractive suspensions. Image analysis algorithms are used to calculate structural and dynamic metrics for the colloidal particles that measure changes due to geometric confinement.

밀폐 무부하 흐르는 콜로이드 중합체 혼합물의 공 촛점 이미징

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed ...

연구

화학

Fabrication of Large-area Free-standing Ultrathin Polymer Films

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films. Typically, ultrathin films are prepared using either sacrificial layers, which may damage the film or affect its mechanical properties, or they are made on freshly cleaved mica, a substrate that is difficult to scale. Further, the size of ultrathin film is typically limited to a few square millimeters. In this method, we modify a surface with a polyelectrolyte that alters the strength of adhesion between polymer and deposition substrate. The polyelectrolyte can be shown to remain on the wafer using spectroscopy, and a treated wafer can be used to produce multiple films, indicating that at best minimal amounts of the polyelectrolyte are added to the film. The process has thus far been shown to be limited in scalability only by the size of the coating equipment, and is expected to be readily scalable to industrial processes. In this study, the protocol for making the solutions, preparing the deposition surface, and producing the films is described.

We describe a method for the fabrication of large-area (up to 13 cm diameter) and ultrathin (as thin as 8 nm) polymer films. Instead of using a sacrificial interlayer to delaminate the film from its substrate, we use a self-limiting surface treatment suitable for arbitrarily large areas.

대 면적의 제작은 초박막 고분자 필름을 무료 서

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films.  Typically, ultrathin films are prepared ...

Photodynamic Therapy with Blended Conducting Polymer/Fullerene Nanoparticle Photosensitizers

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next generation photosensitizers for Photodynamic Therapy (PDT) is reported. The nanoparticles are formed by hydrophobic interaction of the semiconducting polymer MEH-PPV (poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene]) with the fullerene PCBM (phenyl-C61-butyric acid methyl ester) in the presence of a non-compatible solvent. MEH-PPV has a high extinction coefficient that leads to high rates of triplet formation, and efficient charge and energy transfer to the fullerene PCBM. The latter processes enhance the efficiency of the PDT system through fullerene assisted triplet and radical formation, and ultrafast deactivation of MEH-PPV excited stated. The results reported here show that this nanoparticle PDT sensitizing system is highly effective and shows unexpected specificity to cancer cell lines.

This protocol describes a method for the fabrication of conducting polymer nanoparticles blended with fullerene. These nanoparticles were investigated for their potential use as a next generation photosensitizers for Photodynamic Therapy (PDT).

혼합 폴리머 / 풀러렌 나노 입자 감광제를 실시와 광 역학 치료

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next ...

Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step process based on the preparation of a sol in a one-pot synthesis which is followed by the deposition of a gel film on Si(100) substrates by evaporation induced self-assembly using the dip-coating technique and ends with a thermal treatment of the material to induce the gel crystallization and the growth of the quartz film. The formation of a silica gel is based on the reaction of a tetraethyl orthosilicate and water, catalyzed by HCl, in ethanol. However, the solution contains two additional components that are essential for preparing mesoporous epitaxial quartz films from these silica gels dip-coated on Si. Alkaline earth ions, like Sr2+ act as glass melting agents that facilitate the crystallization of silica and in combination with cetyl trimethylammonium bromide (CTAB) amphiphilic template form a phase separation responsible of the macroporosity of the films. The good matching between the quartz and silicon cell parameters is also essential in the stabilization of quartz over other SiO2 polymorphs and is at the origin of the epitaxial growth.

A protocol is presented for the preparation of piezoelectric macroporous epitaxial films of quartz on silicon by solution chemistry using dip-coating and thermal treatments in air.

화학 용액 증착에 의해 실리콘에 거대 다공성 에피 택셜 석영 필름의 제조

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step ...

Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous solution. In a carbon nanotube/PEO105-PPO70-PEO105 (poloxamer 407) aqueous solution, the amphiphilic poloxamer 407 adsorbs onto the carbon nanotube surfaces and self-assembles into continuous layers, driven by intermolecular interactions between constituent molecules. The addition of 5-methylsalicylic acid changes the self-assembled structure from spherical-micellar to a cylindrical morphology. The fabricated poloxamer 407/carbon nanotube hybrid particles exhibit thermo-responsive structural features so that the density and thickness of poloxamer 407 layers are also reversibly controllable by varying temperature. The detailed structural properties of the poloxamer 407/carbon nanotube particles in suspension can be characterized by small-angle neutron scattering experiments and model fit analyses. The distinct curve shapes of the scattering intensities depending on temperature control or addition of aromatic additives are well described by a modified core-shell cylinder model consisting of a carbon nanotube core cylinder, a hydrophobic shell, and a hydrated polymer layer. This method can provide a simple but efficient way for the fabrication and in-situ characterization of carbon nanotube-based nano particles with a structure-tunable encapsulation.

A method for the functionalization of carbon nanotubes with structure-tunable polymeric encapsulation layers and structural characterization using small-angle neutron scattering is presented.

작은 각도 중성자 산란에 의한 열 가역적 블록 공중 합체 및 특성 단일 벽 탄소 나노 튜브의 기능화

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous ...

The Preparation and Properties of Thermo-reversibly Cross-linked Rubber Via Diels-Alder Chemistry

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ethylene-propylene rubber, grafted with maleic anhydride, is thermo-reversibly cross-linked in two steps. The pending anhydride moieties are first modified with furfurylamine to graft furan groups to the rubber backbone. These pendant furan groups are then cross-linked with a bis-maleimide via a Diels-Alder coupling reaction. Both reactions can be performed under a broad range of experimental conditions and can easily be applied on a large scale. The material properties of the resulting Diels-Alder cross-linked rubbers are similar to a peroxide-cured ethylene/propylene/diene rubber (EPDM) reference. The cross-links break at elevated temperatures (&#62; 150 &#176;C) via the retro-Diels-Alder reaction and can be reformed by thermal annealing at lower temperatures (50-70 &#176;C). Reversibility of the system was proven with infrared spectroscopy, solubility tests and mechanical properties. Recyclability of the material was also shown in a practical way, i.e., by cutting a cross-linked sample into small parts and compression molding them into new samples displaying comparable mechanical properties, which is not possible for conventionally cross-linked rubbers.

A simple two-step approach involving rubber modification and cross-linking yields fully reworkable, elastic rubber products.

열 가역적 가교 고무 통해 딜스 - 알더 화학의 준비 및 등록

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ...

Monitoring the Effects of Illumination on the Structure of Conjugated Polymer Gels Using Neutron Scattering

We demonstrate a protocol to effectively monitor the gelation process of a high concentration solution of conjugated polymer both in the presence and absence of white light exposure. By instituting a controlled temperature ramp, the gelation of these materials can be precisely monitored as they proceed through this structural evolution, which effectively mirrors the conditions experienced during the solution deposition phase of organic electronic device fabrication. Using small angle neutron scattering (SANS) and ultra-small angle neutron scattering (USANS) along with appropriate fitting protocols we quantify the evolution of select structural parameters throughout this process. Thorough analysis indicates that continued light exposure throughout the gelation process significantly alters the structure of the ultimately formed gel. Specifically, the aggregation process of poly(3-hexylthiophene-2,5-diyl) (P3HT) nano-scale aggregates is negatively affected by the presence of illumination, ultimately resulting in the retardation of growth in conjugated polymer microstructures and the formation of smaller scale macro-aggregate clusters.

A protocol for the analysis of gels formed from the optoelectronic conjugated polymer poly(3-hexylthiophene-2,5-diyl) (P3HT) using small and ultra-small angle neutron scattering in both the presence and absence of illumination is presented.

중성자 산란을 사용 하 여 활용 된 중합체 젤의 구조에 조명 효과 모니터링

We demonstrate a protocol to effectively monitor the gelation process of a high concentration solution of conjugated polymer both in the presence and ...

Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables the silk proteins to be compact and ordered by shearing and elongation forces. Here, a biomimetic microfluidic channel was designed to mimic the specific geometry of the spinning duct of the silkworm. Regenerated silk fibroin (RSF) spinning doped with high concentration, was extruded through the microchannel to dry-spin fibers at ambient temperature and pressure. In the post-treated process, the as-spun fibers were drawn and stored in ethanol aqueous solution. Synchrotron radiation wide-angle X-ray diffraction (SR-WAXD) technology was used to investigate the microstructure of single RSF fibers, which were fixed to a sample holder with the RSF fiber axis normal to the microbeam of the X-ray. The crystallinity, crystallite size, and crystalline orientation of the fiber were calculated from the WAXD data. The diffraction arcs near the equator of the two-dimensional WAXD pattern indicate that the post-treated RSF fiber has a high orientation degree.

A protocol for the microfluidic spinning and microstructure characterization of regenerated silk fibroin monofilament is presented.

미세 드라이 회전 및 재생성된 실크 Fibroin 섬유의 특성

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables ...

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). ...

Time-resolved Photophysical Characterization of Triplet-harvesting Organic Compounds at an Oxygen-free Environment Using an iCCD Camera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables the acquisition of photoluminescence spectra covering the time regime from nanoseconds up to 0.1 s. This enables us to follow the changes in the intensity (decay) and emission of the spectra over time. Using this method, it is possible to study diverse photophysical phenomena, such as the emission of phosphorescence, and the contributions of prompt and delayed fluorescence in molecules showing thermally activated delayed fluorescence (TADF). Remarkably, all spectra and decays are obtained in a single experiment. This can be done for solids (thin film, powder, crystal) and liquid samples, where the only limitations are the spectral sensitivity of the camera and the excitation wavelength (532 nm, 355 nm, 337 nm, and 266 nm). This technique is, thus, very important when investigating the excited state dynamics in organic emitters for their application in organic light-emitting diodes and other areas where triplet harvesting is of paramount importance. Since triplet states are strongly quenched by oxygen, emitters with efficient TADF luminescence, or those showing room temperature phosphorescence (RTP), must be correctly prepared in order to remove any dissolved oxygen from solutions and films. Otherwise, no long-lived emission will be observed. The method of degassing solid samples as presented in this work is basic and simple, but the degassing of liquid samples creates additional difficulties and is particularly interesting. A method of minimizing solvent loss and changing the sample concentration, while still enabling to remove oxygen in a very efficient and a repeatable manner, is presented in this work.

Here, we present a method of the spectroscopic characterization of organic molecules by means of time-resolved photoluminescence spectroscopy on the nanosecond-to-millisecond timescale in oxygen-free conditions. Methods to efficiently remove oxygen from the samples and, thus, limit luminescence quenching are also described.

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables ...