TCL은 Royal Society Research Grant 2016 R1 (RG150551)과 EPSRC (EP / P511262 / 1)의 기관 후원 상을 통해 자금을 지원 한 UCL BEAMS Future Leader Award의 지원에 감사드립니다. WIKC, TCL 및 IPP는 EPSRC M3S CDT (EP / L015862 / 1)를 통해 A * STAR-UCL 연구 첨부 프로그램이 자금을 지원하는 학생회에 감사드립니다. GD와 TJ는 학생들을 후원해 주신 EPSRC M3S CDT (EP/L015862/1)에 감사드립니다. TJ와 TCL은 TJ의 학생들에 기여한 Camtech Innovations를 인정합니다. 모든 저자는 UCL Open Access Fund에 감사드립니다.

1. Au NPs의 합성
<ol><li>종래의 투르케비치 방법을 통한 Au 종자의 합성26<ol>
<li>98.5 mg의 HAuCl4· 3H2O전구체와 유리 바이알에 탈이온수 10 mL. 참고: 소량의 HAuCl4 전구체를 계량 보트로 옮기고 HAuCl4 전구체가 금속 실험실을 부식시키기 때문에 금속 주걱 대신 플라스틱 주걱을 사용하여 결정을 계량합니다. HAuCl4는 흡습성이므로 가능한 한 신속하게 칭량 단계를 수행해야하므로 대기에서 물을 흡수하여 시간이 지남에 따라 무게가 증가합니다. HAuCl4는 부식성이 강하고 심한 피부 화상과 눈 손상을 일으킬 수 있습니다. 그것을 취급 할 때 특별한주의를 기울이십시오.</li>
		<li>구연산나트륨 분말 64.5 mg을 유리 바이알에 탈이온수 0.5 mL와 함께 용해시켜 500 mM 시트르산나트륨 용액 0.5 mL를 제조하였다.</li>
		<li>25 mM HAuCl4 용액 1 mL를 250 mL 청색 캡핑된 병에 99 mL의 물로 희석하여 0.25 mM HAuCl4 용액 100 mL를 수득하였다.</li>
		<li>0.25 mM HAuCl4 용액 99.5 mL를 콘덴서가 장착된 250 mL 삼구 둥근 바닥 플라스크에 첨가한다. 용액을 격렬한 교반 하에 90°C로 가열하고 15분 동안 온도를 유지한다.</li>
		<li>500 mM 시트르산 나트륨 용액 0.5 mL를 반응 혼합물에 주입하고 온도를 유지하고 용액의 색이 루비 레드로 변할 때까지 교반한다. 참고 : 반응은 약 30 분이 걸립니다.</li>
	</ol></li>
	<li>운동학적으로 조절된 방법13을 통한 Au NPs의 시딩된 성장
	<ol>
<li>합성된 Au 시드 용액을 70°C로 냉각시킨다.</li>
		<li>10 mL의 시트르산나트륨 분말 154.8 mg을 유리 바이알에 탈이온수 10 mL와 함께 용해시켜 60 mM 시트르산나트륨 용액을 준비한다.</li>
		<li>0.67 mL의 25 mM HAuCl4 용액 및 0.67 mL의 60 mM 시트르산나트륨 용액을 2분의 시간 간격으로 Au 종자에 주입한다.</li>
		<li>단계 1.2.3을 반복하여 Au NP의 크기를 점진적으로 40nm로 증가시킨다. 참고 : 40nm에 도달하려면 약 10 개의 성장 단계가 필요합니다. 필요한 실제 단계 수는 정확한 설정에 따라 달라질 수 있습니다.</li>
	</ol></li>
	<li>자동 합성기를 사용한 Au NP의 시드 성장(그림 2)
	<ol>
<li>섹션 1에서 제조된 Au 시드 용액 25 mL를 50 mL 원뿔형 원심분리 튜브로 옮기고 열믹서에서 70°C로 냉각시킨다. 참고: 물 25mL가 들어있는 50mL 원심분리 튜브에 넣은 열전대 온도계를 사용하여 열전대 온도계를 사용하여 열믹서 내부의 온도를 모니터링하십시오.</li>
		<li>3 mL 루어락 일회용 주사기를 2.5 mL의 25 mM HAuCl4 용액으로 채운다. 또 다른 3 mL 루어락 일회용 주사기를 2.5 mL의 60 mM 소듐 시트레이트 용액으로 채운다.</li>
		<li>주사기를 시린지 펌프에 넣고 Luer-to-MicroTight 어댑터를 사용하여 PEEK 튜브(150μm 내부 직경)를 주사기에 연결합니다. 튜빙을 열믹서 내의 Au 시드 용액을 포함하는 원심분리 튜브에 삽입한다.</li>
		<li>두 시린지 펌프를 모두 설정하여 0.1675mL의 용액을 20분에 걸쳐 분배합니다(분당 8.357μL).</li>
		<li>써모믹서 회전 속도를 700rpm으로 설정하고 25mM HAuCl4 용액이 포함된 시린지 펌프에서 시작을 누릅니다.</li>
		<li>2분 후, 60 mM 시트르산나트륨 용액을 함유하는 시린지 펌프 상에서 시작 을 누른다.</li>
		<li>HAuCl4 용액 주입을 시작한 지 30분 후, 분석을 위해 Au NP 용액의 분취량을 제거하였다.</li>
		<li>1.3.5 – 1.3.7단계를 반복하여 Au NP의 직경을 최대 40nm까지 점진적으로 늘립니다. 참고: 이 설정은 1.3.4단계에서 추가된 반응물의 부피를 증가시켜 한 단계에서 Au NP를 최대 40nm까지 성장시키는 데 사용할 수 있습니다. 이것은 동일한 주사 속도를 유지하면서 분배 시간을 증가시킴으로써 달성됩니다.</li>
	</ol></li>
</ol>2. Au NP의 특성화
<ol><li>UV-Vis 분광법<ol>
<li>Au NP 용액 1 mL를 세미 마이크로 석영 큐벳에 첨가한다.</li>
		<li>분광계를 켭니다.</li>
		<li>파장 범위를 400 - 800 nm로 설정합니다.</li>
		<li>각 샘플에 대한 UV-Vis 스펙트럼을 획득한다.</li>
	</ol>
</li>
	<li>동적 광산란(DLS)<ol>
<li>샘플 용액을 0.22 μm 필터가 있는 플라스틱 세미 마이크로 큐벳으로 필터링합니다.</li>
		<li>DLS 계측기를 켭니다.</li>
		<li>온도를 25°C로 설정하고 60초 동안 평형을 이룹니다.</li>
		<li>각 샘플의 유체역학적 크기를 측정합니다.</li>
	</ol>
</li>
	<li>투과 전자 현미경 (TEM)<ol>
<li>샘플 용액의 5 μL 액적을 C-코팅된 300-메쉬 Cu 그리드 상에 드롭-캐스팅하고 공기 중에서 건조시킨다. 참고: 희석은 TEM 그리드 상에 잘 분산된 Au NP를 얻기 위해 더 농축된 Au NP 용액 샘플을 위해 필요하다.</li>
		<li>200kV 가속 전압에서 TEM을 사용하여 각 샘플에 대해 여러 TEM 이미지를 획득합니다.</li>
		<li>ImageJ를 사용하여 각 샘플에 대한 200Au NP의 직경을 측정하여 평균 크기 및 표준 편차를 계산합니다.</li>
	</ol>
</li>
</ol>3. CB7-UA 복합체의 형성
<ol><li>0.4 mM CB7 용액의 제조<ol>
<li>4.65 mg의 CB7을 15 mL 유리 바이알에 첨가하십시오. 참고 : CB7의 양은 문헌의 대부분의 보고서에 의해 사용 된 CB7 (= 1163 Da)의 공식 중량을 기준으로 계산됩니다. 그럼에도 불구하고 CB7 고체 샘플은 일반적으로 합성 및 정제 단계에서 남아있는 물, HCl, 메탄올 및 기타 염을 함유하여 샘플에서 ~ 10 - 20 %의 죽은 중량에 기여합니다. 포획된 용매 및 염은 진공 오븐 또는 다른 수단에서 가열함으로써 제거될 수 없었다. 그들의 양은 샘플의 다른 배치에 따라 다르지만 원소 분석을 사용하여 정량화 할 수 있습니다. 그러나, 제시된 프로토콜은 CB7 샘플 내의 용매 및 염의 정량화되지 않은 양의 존재에 민감하지 않다.</li>
		<li>바이알에 물 10mL를 넣고 뚜껑을 조이십시오.</li>
		<li>CB7 고체가 완전히 용해 될 때까지 실온에서 샘플을 초음파 처리하십시오. 참고: CB7은 문헌27 에 따라 합성되었지만 상업적으로 입수가능하다.</li>
	</ol>
</li>
	<li>0.4 mM UA 용액의 제조<ol>
<li>2.69 mg의 UA를 50 mL 원심분리 튜브에 첨가한다.</li>
		<li>튜브에 물 40mL를 넣고 뚜껑을 조이십시오.</li>
		<li>열믹서를 사용하여 온도를 70°C, 속도를 800rpm, 시간을 2h로 설정하여 시료 용액을 소용돌이친다. 용액을 실온으로 식히십시오. 참고: UA는 물에 대한 용해도가 낮음(0.40 mM)5. UA 분말이 완전히 용해되지 않은 경우 더 오래 소용돌이치십시오. 대안적으로, 초음파는 용해를 용이하게 하기 위해 사용될 수 있다.</li>
	</ol>
</li>
	<li>0.4 mM UA 용액의 순차적 희석<ol>
<li>0.4 mM UA 용액 5 mL를 15 mL 유리 바이알에 물 5 mL로 희석하여 0.2 mM UA 용액 10 mL를 수득하였다. 뚜껑을 조이고 30 초 동안 초음파 처리하십시오.</li>
		<li>표 1에 설명된 대로 적절한 양의 UA 및 물을 사용하여 3.3.1단계를 반복합니다.</li>
	</ol>
</li>
	<li>CB7-UA 복합체의 제조<ol>
<li>0.75 mL의 0.4 mM CB7 용액 및 0.75 mL의 0.4 mM UA 용액을 1.5 mL 튜브에 첨가한다. 뚜껑을 고정하고 30 초 동안 초음파 처리하십시오.</li>
		<li>호스트 - 게스트 단지의 형성을 보장하기 위해 30 분 동안 기다리십시오.</li>
		<li>농도가 다른 UA 솔루션을 사용하여 3.4.1 – 3.4.2 단계를 반복합니다.</li>
	</ol>
</li>
</ol>4. UA의 SERS 감지
<ol><li>라만 시스템의 실험 설정(그림 3)<ol>
<li>633nm He-Ne 레이저(22.5mW)를 켭니다.</li>
		<li>모듈식 라만 분광계를 켭니다.</li>
		<li>컴퓨터를 켜고 소프트웨어를 시작합니다.</li>
		<li>분광기 응용 프로그램 마법사 아이콘을 클릭한 다음 Raman을 선택합니다.</li>
		<li>새로운 인수를 시작하십시오. 통합 시간을 30초로 설정하고, 스캔을 평균으로 5초로, 박스카를 0으로 설정합니다.</li>
		<li>배경 스펙트럼을 저장하고 레이저 파장(즉, 633nm)을 입력합니다. 참고: 통합 시간은 각 스캔의 시간이며, 평균에 대한 스캔은 각 스펙트럼을 만들기 위해 평균화된 스캔 수이며, boxcar는 평균28개의 인접 픽셀 수입니다.</li>
	</ol>
</li>
	<li>SERS 기판의 형성<ol>
<li>0.9 mL의 40 nm Au NP 용액 및 0.1 mL의 예비-형성된 CB7-UA 복합체 용액을 1.5 mL 튜브에 첨가한다. 뚜껑을 고정하고 용액이 루비 레드에서 보라색으로 바뀔 때까지 초음파 처리하십시오. 참고: 상업적인 시트레이트-안정화된 40 nm Au NP 용액 샘플이 또한 사용될 수 있다. 전형적으로, 국부적인 표면 플라즈몬 공명 (LSPR) 피크의 광학 밀도는 농축된 원액 샘플로부터의 희석을 통해 1로 조정된다. 샘플 중의 시트레이트 농도는 전형적으로 2 mM로 유지된다.</li>
		<li>샘플 용액을 세미 마이크로 큐벳으로 옮깁니다. 큐벳을 라만 샘플 홀더에 넣고 덮개를 닫습니다.</li>
		<li>측정을 시작합니다.</li>
		<li>자동 저장을 설정하여 다섯 개의 연속 SERS 스펙트럼을 기록합니다.</li>
		<li>측정을 중지하고 샘플을 변경합니다.</li>
		<li>다양한 농도의 CB7-UA 용액을 사용하여 4.2.1 – 4.2.5 단계를 반복하십시오. 참고: 응집 시간은 Au NP의 응집을 매개하는 데 큰 기여를 하는 빈 CB7의 농도의 차이로 인해 0.1 μM UA의 경우 30 초에서 20 μM UA의 경우 30분에 이르는 나노응집체 내의 UA의 농도에 의존하는 것으로 밝혀졌다. CB7-UA 복합체의 경우, 하나의 포털은 부피가 큰 UA 분자에 의해 차단되어, Au NP 표면에 결합하는 것을 사용할 수 없게 되고, 따라서 NP 응집(21)을 매개할 수 없게 된다. 샘플은 용액의 색상이 루비 레드에서 보라색으로 변할 때 측정 할 준비가되었습니다.</li>
	</ol>
</li>
</ol>5. 데이터 분석
<ol><li>데이터 처리<ol>
<li>비대칭 최소 제곱(ALS) 플러그인을 사용하여 베이스라인을 다운로드하여 Origin에 설치합니다. 참고: ALS 플러그인에는 OriginPro가 필요합니다.</li>
		<li>원시 데이터를 원본에 삽입합니다.</li>
		<li>각 샘플의 다섯 SERS 스펙트럼에서 평균값을 계산합니다. 값을 레이저의 힘(즉, 22.5mW)과 통합 시간(즉, 30초)으로 나눕니다.</li>
		<li>ALS 아이콘을 클릭하여 대화 상자를 엽니다. 비대칭 계수를 0.001로, 임계값을 0.03%로, 평활 계수를 2로, 반복 횟수를 20으로 설정하여 각 평균 스펙트럼의 기준선을 수정합니다.</li>
		<li>y 오프셋으로 누적된 선을 사용하여 다른 UA 농도의 SERS 스펙트럼을 플로팅합니다. 출력은 라만 시프트 (cm-1)에 대한 강도 (카운트 s-1 mW-1)이어야합니다.</li>
	</ol>
</li>
</ol>

<ol>
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저자는 공개 할 것이 없습니다.

프로토콜에 설명된 자동화된 합성 방법을 통해 크기가 증가하는 Au NP를 재현 가능하게 합성할 수 있습니다. 종자 합성 중에 구연산 나트륨을 빠르게 첨가하고 PEEK 튜브가 안전한지 확인하기 위해 주기적으로 검사하는 것과 같이 수동으로 수행해야하는 몇 가지 요소가 있지만,이 방법을 사용하면 일반적으로 HAuCl4 및 구연산 나트륨을 여러 번 수동으로 주입해야하는 큰 크기 (최대40nm )의 Au ...

퓨린 뉴클레오티드의 신진 대사의 최종 산물 인 요산은 통풍, 자간전증, 신장 질환, 고혈압, 심혈관 질환 및 당뇨병 1,2,3,4,5와 같은 질병의 진단을위한 혈액 혈청 및 소변의 중요한 바이오 마커입니다. 요산 검출을위한 현재의 방법에는 비색 효소 분석, 고성능 액체 크로마토그래피 및 모세관 전기 영동이 포함되며, 이는 시간이 많이 걸리고 비용이 많이 들며 정교한 샘플 준비 6,7,8,9가 필요합니다.
표면 강화 라만 분광법은 진동 지문을 통해 생체 분자를 선택적으로 검출 할 수 있고 고감도, 신속한 반응, 사용 편의성 및 시료 준비 없음 또는 최소와 같은 수많은 이점을 제공하므로 일상적인 진료 시점 진단을위한 유망한 기술입니다. 귀금속 나노입자(예를 들어, Au NPs)에 기초한 SERS 기판은 표면 플라즈몬 공명(11)에 의해 야기된 강한 전자기 향상을 통해 분석물 분자의 라만 신호를 크기10의 4 내지10 차수만큼 향상시킬 수 있다. 맞춤형 크기의 Au NP는 복잡한 금속 나노복합체(12)의 제조에 시간이 많이 걸리는 것과는 달리 쉽게 합성될 수 있으며, 따라서 이들의 우수한 특성(13,14,15,16)으로 인해 생물 의학 응용에 널리 사용된다. Au NPs의 표면 상에 거대고리 분자인 cucurbit[n]urils(CBn, 여기서 n=5-8, 10)의 부착은 고도로 대칭적이고 단단한 CB 분자가 Au NP 사이의 정확한 간격을 제어하고 숙주-게스트 복합체의 형성을 통해 플라즈몬 핫스팟에 중심 또는 근접하게 분석물 분자를 국부화할 수 있기 때문에 분석물 분자의 SERS 신호를 더욱 강화할 수 있다(도 1)17, 18,19,20. Au NP를 사용한 SERS 연구의 이전 예: CBn 나노응집체에는 니트로폭발물, 다환식 방향족제, 디아미노스틸벤, 신경전달물질 및 크레아티닌 21,22,23,24,25 가 포함되며, SERS 측정은 큐벳에서 수행되거나 맞춤형 샘플 홀더에 작은 물방울을 적재하여 수행됩니다. 이러한 검출 스킴은 높은 재현성을 갖는 복잡한 매트릭스에서 바이오마커를 신속하게 정량화하는데 특히 유용하다.
본원에서, CB7 및 중요한 바이오마커 UA의 숙주-게스트 복합체를 형성하고, 수성 매질에서 Au NPs의 CB7 매개된 응집을 통해 0.2 μM의 검출 한계로 UA를 정량화하는 용이한 방법이 모듈형 분광계를 사용하여 입증되었으며, 이는 진단 및 임상 적용에 유망하다.

<table>
	<tbody>
		<tr>
			<td>40 nm gold nanoparticles</td>
			<td>NanoComposix</td>
			<td>AUCN40-100M</td>
			<td>NanoXact, 0.05 mg/ mL, bare (citrate)</td>
		</tr>
		<tr>
			<td>Centrifuge tube</td>
			<td>Corning Falcon</td>
			<td>14-432-22</td>
			<td>50 mL volume</td>
		</tr>
		<tr>
			<td>Cucurbit[7]uril</td>
			<td>Lab-made</td>
			<td></td>
			<td>see ref. 19</td>
		</tr>
		<tr>
			<td>Gold(III) chloride trihydrate</td>
			<td>Sigma aldrich</td>
			<td>520918</td>
			<td>&#8805;99.9% trace metals basis</td>
		</tr>
		<tr>
			<td>Luer lock disposable syringe</td>
			<td>Cole-Parmer</td>
			<td>WZ-07945-15</td>
			<td>3 mL volume</td>
		</tr>
		<tr>
			<td>Luer-to-MicroTight adapter</td>
			<td>LuerTight</td>
			<td>P-662</td>
			<td>360 &#956;m outer diameter Tubing to Luer Syringe</td>
		</tr>
		<tr>
			<td>PEEK tubing</td>
			<td>IDEX</td>
			<td>1572</td>
			<td>360 &#956;m outer diameter, 150 &#956;m inner diameter</td>
		</tr>
		<tr>
			<td>PEEK tubing cutter</td>
			<td>IDEX</td>
			<td>WZ-02013-30</td>
			<td>Capillary Polymer Chromatography Tubing Cutter For 360 &#181;m to 1/32&#34; OD tubing</td>
		</tr>
		<tr>
			<td>Raman spectrometer</td>
			<td>Ocean Optics</td>
			<td>QE pro</td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium citrate tribasic dihydrate</td>
			<td>Sigma aldrich</td>
			<td>S4641</td>
			<td>ACS reagent, &#8805;99.0%</td>
		</tr>
		<tr>
			<td>Sonicator</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Standard Probe</td>
			<td>Digi-Sense</td>
			<td>WZ-08516-55</td>
			<td>Type-K</td>
		</tr>
		<tr>
			<td>Syringe pump</td>
			<td>Aladdin</td>
			<td>ALADDIN2-220</td>
			<td>2 syringes, maximum syringe volume 60 mL</td>
		</tr>
		<tr>
			<td>Thermocouple thermometer</td>
			<td>Digi-Sense</td>
			<td>WZ-20250-91</td>
			<td>Single-Input Thermocouple Thermometer with NIST-Traceable Calibration</td>
		</tr>
		<tr>
			<td>ThermoMixer</td>
			<td>Eppendorf</td>
			<td>5382000031</td>
			<td>With an Eppendorf SmartBlock for 50 mL tubes</td>
		</tr>
		<tr>
			<td>Uric acid</td>
			<td>Sigma aldrich</td>
			<td>U2625</td>
			<td>&#8805;99%, crystalline</td>
		</tr>
	</tbody>
</table>

quantitative sers detection of uric acid via formation of precise plasmonic nanojunctions within aggregates of gold nanoparticles and cucurbit[n]uril

이 연구는 모듈형 분광계를 사용하여 지문 영역의 여러 특성 피크에 대해 ~0.2μM의 낮은 검출 한계로 표면 강화 라만 분광법(SERS)을 통해 중요한 바이오마커인 요산(UA)의 정량적 검출을 위한 신속하고 매우 민감한 방법을 설명합니다. 이러한 바이오센싱 기법은 매크로사이클, cucurbit[7]uril (CB7) 및 UA 사이의 숙주-게스트 복합체화에 의해 매개되고, 이후 자체 조립된 Au NP:CB7 나노응집체 내에서 정확한 플라즈몬 나노접합의 형성에 의해 매개된다. SERS 기질에 대해 바람직한 크기의 용이한 Au NP 합성은 또한 실험실에서 제작한 자동 합성기를 사용하여 촉진될 수 있는 옵션을 갖는 고전적인 시트레이트 환원 접근법에 기초하여 수행되었다. 이 프로토콜은 임상 적용을 위해 체액에서 바이오마커의 다중화 검출로 쉽게 확장될 수 있다.

제시된 Au NP 합성에서 UV-Vis 스펙트럼은 10 성장 단계 (그림 4 A, B) 후에 LSPR 피크의 521 nm에서 529 nm로 이동을 보여 주며 DLS 데이터는 Au NP의 크기가 25.9 nm에서 42.8 nm로 증가함에 따라 좁은 크기 분포를 보여줍니다 (그림 4C, D). TEM 이미지에서 측정된 G0, G5 및 G10의 평균 크기(그림 4E)는 각각 20.1nm, 2.1nm± 32.5nm, 40.0...

Watch this Scientific Journal Video about Quantitative SERS Detection of Uric Acid via Formation of Precise Plasmonic Nanojunctions within Aggregates of Gold Nanoparticles and Cucurbit[n]uril at JoVE.

Quantitative SERS Detection of Uric Acid via Formation of Precise Plasmonic Nanojunctions within Aggregates of Gold Nanoparticles and Cucurbit[n]uril

큐커빗[7]우릴 및 요산의 호스트-게스트 복합체를 Au NP 용액에 소량 첨가하기 전에 수용액에서 형성하여 모듈형 분광계를 이용한 정량적 표면 강화 라만 분광법(SERS) 감지를 수행하였다.

금 나노 입자와 Cucurbit[n]uril의 응집체 내에서 정확한 플라즈몬 나노 접합의 형성을 통한 요산의 정량적 SERS 검출

This work describes a rapid and highly sensitive method for the quantitative detection of an important biomarker, uric acid (UA), via surface-enhanced ...

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Research

JoVE Journal

Chemistry

Quantitative SERS Detection of Uric Acid via Formation of Precise Plasmonic Nanojunctions within Aggregates of Gold Nanoparticles and Cucurbit[n]uril

3.7K 조회수.  University College London (UCL). 큐커빗[7]우릴 및 요산의 호스트-게스트 복합체를 Au NP 용액에 소량 첨가하기 전에 수용액에서 형성하여 모듈형 분광계를 이용한 정량적 표면 강화 라만 분광법(SERS) 감지를 수행하였다.

비디오: Quantitative SERS Detection of Uric Acid via Formation of Precise Plasmonic Nanojunctions within Aggregates of Gold Nanoparticles and Cucurbit[n]uril

Template Directed Synthesis of Plasmonic Gold Nanotubes with Tunable IR Absorbance

A nearly parallel array of pores can be produced by anodizing aluminum foils in acidic environments1, 2. Applications of anodic aluminum oxide (AAO) membranes have been under development since the 1990's and have become a common method to template the synthesis of high aspect ratio nanostructures, mostly by electrochemical growth or pore-wetting. Recently, these membranes have become commercially available in a wide range of pore sizes and densities, leading to an extensive library of functional nanostructures being synthesized from AAO membranes. These include composite nanorods, nanowires and nanotubes made of metals, inorganic materials or polymers 3-10. Nanoporous membranes have been used to synthesize nanoparticle and nanotube arrays that perform well as refractive index sensors, plasmonic biosensors, or surface enhanced Raman spectroscopy (SERS) substrates 11-16, as well as a wide range of other fields such as photo-thermal heating 17, permselective transport 18, 19, catalysis 20, microfluidics 21, and electrochemical sensing 22, 23. Here, we report a novel procedure to prepare gold nanotubes in AAO membranes. Hollow nanostructures have potential application in plasmonic and SERS sensing, and we anticipate these gold nanotubes will allow for high sensitivity and strong plasmon signals, arising from decreased material dampening 15.

Solution-suspendable gold nanotubes with controlled dimensions can be synthesized by electrochemical deposition in porous anodic aluminum oxide (AAO) membranes using a hydrophobic polymer core. Gold nanotubes and nanotube arrays hold promise for applications in plasmonic biosensing, surface-enhanced Raman spectroscopy, photo-thermal heating, ionic and molecular transport, microfluidics, catalysis and electrochemical sensing.

템플릿 조정할 IR의 흡광도와 Plasmonic 골드 나노 튜브의 합성을 감독

A nearly parallel array of pores can be produced by anodizing aluminum foils in acidic environments1, 2. Applications of anodic aluminum oxide (AAO) ...

연구

화학

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan &#948; solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials&#39; morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by St&#246;ber&#39;s methods, which have smooth surfaces.

Silica nanoparticles were prepared using acid-catalysis of a siloxane precursor and microwave-assisted synthetic techniques resulting in the controlled growth of nanomaterials ranging from 30-250 nm in diameter. The growth dynamics can be controlled by varying the initial silicic acid concentration, time of the reaction, and temperature of reaction.

전자 레인지를 이용한 산 - 촉매 반응을 통해 실리카 나노 입자의 제조

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

A Simple Method for the Size Controlled Synthesis of Stable Oligomeric Clusters of Gold Nanoparticles under Ambient Conditions

Reducing dilute aqueous HAuCl4 with sodium thiocyanate (NaSCN) under alkaline conditions produces 2 to 3 nm diameter nanoparticles. Stable grape-like oligomeric clusters of these yellow nanoparticles of narrow size distribution are synthesized under ambient conditions via two methods. The delay-time method controls the number of subunits in the oligoclusters by varying the time between the addition of HAuCl4 to alkaline solution and the subsequent addition of reducing agent, NaSCN. The yellow oligoclusters produced range in size from ~3 to ~25 nm. This size range can be further extended by an add-on method utilizing hydroxylated gold chloride (Na+[Au(OH4-x)Clx]-) to auto-catalytically increase the number of subunits in the as-synthesized oligocluster nanoparticles, providing a total range of 3 nm to 70 nm. The crude oligocluster preparations display narrow size distributions and do not require further fractionation for most purposes. The oligoclusters formed can be concentrated &#62;300 fold without aggregation and the crude reaction mixtures remain stable for weeks without further processing. Because these oligomeric clusters can be concentrated before derivatization they allow expensive derivatizing agents to be used economically. In addition, we present two models by which predictions of particle size can be made with great accuracy.

We describe a simple method for producing highly stable oligomeric clusters of gold nanoparticles via the reduction of chloroauric acid (HAuCl4) with sodium thiocyanate (NaSCN). The oligoclusters have a narrow size distribution and can be produced with a wide range of sizes and surface coats.

주변 조건에 따라 금 나노 입자의 안정 올리고머 클러스터의 크기 제어 합성을위한 간단한 방법

Reducing dilute aqueous HAuCl4 with sodium thiocyanate (NaSCN) under alkaline conditions produces 2 to 3 nm diameter nanoparticles. Stable grape-like ...

Synthesis of Ligand-free CdS Nanoparticles within a Sulfur Copolymer Matrix

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature solvents. These coordinating ligands help solubilize and stabilize the nanoparticles while in solution, and can influence the resulting size and reactivity of the nanoparticles during their formation. Despite the ubiquity of using ligands during synthesis, the presence of aliphatic ligands on the nanoparticle surface can result in a number of problems during the end use of the nanoparticles, necessitating further ligand stripping or ligand exchange procedures. We have developed a way to synthesize cadmium sulfide (CdS) nanoparticles using a unique sulfur copolymer. This sulfur copolymer is primarily composed of elemental sulfur, which is a cheap and abundant material. The sulfur copolymer has the advantages of operating both as a high temperature solvent and as a sulfur source, which can react with a cadmium precursor during nanoparticle synthesis, resulting in the generation of ligand free CdS. During the reaction, only some of the copolymer is consumed to produce CdS, while the rest remains in the polymeric state, thereby producing a nanocomposite material. Once the reaction is finished, the copolymer stabilizes the nanoparticles within a solid polymeric matrix. The copolymer can then be removed before the nanoparticles are used, which produces nanoparticles that do not have organic coordinating ligands. This nascent synthesis technique presents a method to produce metal-sulfide nanoparticles for a wide variety of applications where the presence of organic ligands is not desired.

Herein we present a method to synthesize ligand-free cadmium sulfide (CdS) nanoparticles based on a unique sulfur copolymer. The sulfur copolymer operates as a high temperature solvent and a sulfur source during the nanoparticle synthesis and stabilizes the nanoparticles after the reaction.

황 합체 매트릭스 내의 자유 리간드의 CDS 나노 입자의 합성

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature ...

An Optimized Protocol for the Efficient Radiolabeling of Gold Nanoparticles by Using a 125I-labeled Azide Prosthetic Group

Here, we demonstrate a detailed protocol for the radiosynthesis of a 125I-labeled azide prosthetic group and its application to the efficient radiolabeling of DBCO-group-functionalized gold nanoparticles using a copper-free click reaction. Radioiodination of the stannylated precursor (2) was carried out by using [125I]NaI and chloramine T as an oxidant at room temperature for 15 min. After HPLC purification of the crude product, the purified 125I-labeled azide (1) was obtained with high radiochemical yield (75 &plusmn; 10%, n = 8) and excellent radiochemical purity (&gt;99%). For the synthesis of radiolabeled 13-nm-sized gold nanoparticles, the DBCO-functionalized gold nanoparticles (3) were prepared by using a thiolated polyethylene glycol polymer. A copper-free click reaction between 1 and 3 gave the 125I-labeled gold nanoparticles (4) with more than 95% of radiochemical yield as determined by radio-thin-layer chromatography (radio-TLC). These results clearly indicate that the present radiolabeling method using a strain-promoted copper-free click reaction will be useful for the efficient and convenient radiolabeling of DBCO-group-containing nanomaterials.

An Optimized Protocol for the Efficient Radiolabeling of Gold Nanoparticles by Using a 125I-labeled Azide Prosthetic Group

A detailed procedure for the synthesis of a 125I-labeled azide and the radiolabeling of dibenzocyclooctyne (DBCO)-group-conjugated, 13-nm-sized gold nanoparticles using a copper-free click reaction is described.

를 사용하여 금 나노 입자의 효율적인 방사성 표지를위한 최적화 된 프로토콜<sup&gt; (125)</sup&gt; I-표시 아 지드 보철 그룹

Here, we demonstrate a detailed protocol for the radiosynthesis of a 125I-labeled azide prosthetic group and its application to the efficient ...

Luminophore Formation in Various Conformations of Bovine Serum Albumin by Binding of Gold(III)

The purpose of the presented protocols is to study the process of Au(III) binding to BSA, yielding conformation change-induced red fluorescence (&#955;em = 640 nm) of BSA-Au(III) complexes. The method adjusts the pH to show that the emergence of the red fluorescence is correlated with the pH-induced equilibrium transitions of the BSA conformations. Red fluorescent BSA-Au(III) complexes can only be formed with an adjustment of pH at or above 9.7, which corresponds to the &#34;A-form&#34; conformation of BSA. The protocol to adjust the BSA to Au molar ratio and to monitor the time-course of the process of Au(III) binding is described. The minimum number of Au(III) per BSA, to produce the red fluorescence, is less than seven. We describe the protocol in steps to illustrate the presence of multiple Au(III) binding sites in BSA. First, by adding copper (Cu(II)) or nickel (Ni(II)) cations followed by Au(III), this method reveals a binding site for Au(III) that is not the red fluorophore. Second, by modifying BSA by thiol capping agents, another nonfluorophore-forming Au(III) binding site is revealed. Third, changing the BSA conformation by cleaving and capping of the disulfide bonds, the possible Au(III) binding site(s) are illustrated. The protocol described, to control the BSA conformations and Au(III) binding, can be generally applied to study the interactions of other proteins and metal cations.

Luminophore Formation in Various Conformations of Bovine Serum Albumin by Binding of GoldIII

The protocols for studying the binding of gold cations (Au(III)) to various conformations of bovine serum albumin (BSA) as well as for characterizing the conformational dependent unique BSA-Au fluorescence are presented.

Gold(III)의 바인딩에 의해 소 혈 청 알 부 민의 다양 한 Conformations에 Luminophore 형성

The purpose of the presented protocols is to study the process of Au(III) binding to BSA, yielding conformation change-induced red fluorescence (&#955;em ...

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.

합성 및 암화 금 나노 입자의 특성화

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

Assembly of Gold Nanorods into Chiral Plasmonic Metamolecules Using DNA Origami Templates

The inherent addressability of DNA origami structures makes them ideal templates for the arrangement of metal nanoparticles into complex plasmonic nanostructures. The high spatial precision of a DNA origami-templated assembly allows controlling the coupling between plasmonic resonances of individual particles and enables tailoring optical properties of the constructed nanostructures. Recently, chiral plasmonic systems attracted a lot of attention due to the strong correlation between the spatial configuration of plasmonic assemblies and their optical responses (e.g., circular dichroism [CD]). In this protocol, we describe the whole workflow for the generation of DNA origami-based chiral assemblies of gold nanorods (AuNRs). The protocol includes a detailed description of the design principles and experimental procedures for the fabrication of DNA origami templates, the synthesis of AuNRs, and the assembly of origami-AuNR structures. In addition, the characterization of structures using transmission electron microscopy (TEM) and CD spectroscopy is included. The described protocol is not limited to chiral configurations and can be adapted for the construction of various plasmonic architectures.

We describe the detailed protocol for the DNA origami-based assembly of gold nanorods into chiral plasmonic metamolecules with strong chiroptical responses. The protocol is not limited to chiral configurations and can be easily adapted for the fabrication of various plasmonic architectures.

DNA 종이 접기 서식 파일을 사용 하 여 키 랄 Plasmonic Metamolecules로 금 Nanorods의 조립

The inherent addressability of DNA origami structures makes them ideal templates for the arrangement of metal nanoparticles into complex plasmonic ...

Performing Spectroscopy on Plasmonic Nanoparticles with Transmission-Based Nomarski-Type Differential Interference Contrast Microscopy

Differential interference contrast (DIC) microscopy is a powerful imaging tool that is most commonly employed for imaging microscale objects using visible-range light. The purpose of this protocol is to detail a proven method for preparing plasmonic nanoparticle samples and performing single particle spectroscopy on them with DIC microscopy. Several important steps must be followed carefully in order to perform repeatable spectroscopy experiments. First, landmarks can be etched into the sample substrate, which aids in locating the sample surface and in tracking the region of interest during experiments. Next, the substrate must be properly cleaned of debris and contaminants that can otherwise hinder or obscure examination of the sample. Once a sample is properly prepared, the optical path of the microscope must be aligned, using Kohler Illumination. With a standard Nomarski style DIC microscope, rotation of the sample may be necessary, particularly when the plasmonic nanoparticles exhibit orientation-dependent optical properties. Because DIC microscopy has two inherent orthogonal polarization fields, the wavelength-dependent DIC contrast pattern reveals the orientation of rod-shaped plasmonic nanoparticles. Finally, data acquisition and data analyses must be carefully performed. It is common to represent DIC-based spectroscopy data as a contrast value, but it is also possible to present it as intensity data. In this demonstration of DIC for single particle spectroscopy, the focus is on spherical and rod-shaped gold nanoparticles.

The goal of this protocol is to detail a proven approach for the preparation of plasmonic nanoparticle samples and for performing single particle spectroscopy on them with differential interference contrast (DIC) microscopy.

투과 형 Nomarski 타입 차동 간섭 콘트라스트 현미경을 사용 하 여 플라스 몬 Ic 나노 입자에 대 한 분광학 수행

Differential interference contrast (DIC) microscopy is a powerful imaging tool that is most commonly employed for imaging microscale objects using ...

Synthesis of Aptamer-PEI-g-PEG Modified Gold Nanoparticles Loaded with Doxorubicin for Targeted Drug Delivery

Due to drug resistance and toxicity in healthy cells, use of doxorubicin (DOX) has been limited in clinical cancer therapy. This protocol describes the designing of poly(ethylenimine) grafted with polyethylene glycol (PEI-g-PEG) copolymer functionalized gold nanoparticles (AuNPs) with loaded aptamer (AS1411) and DOX through amide reactions. AS1411 is specifically bonded with targeted nucleolin receptors on cancer cells so that DOX targets cancer cells instead of healthy cells. First, PEG is carboxylated, then grafted to branched PEI to obtain a PEI-g-PEG copolymer, which is confirmed by 1H NMR analysis. Next, PEI-g-PEG copolymer coated gold nanoparticles (PEI-g-PEG@AuNPs) are synthesized, and DOX and AS1411 are covalently bonded to AuNPs gradually via amide reactions. The diameter of the prepared AS1411-g-DOX-g-PEI-g-PEG@AuNPs is ~39.9 nm, with a zeta potential of -29.3 mV, indicating that the nanoparticles are stable in water and cell medium. Cell cytotoxicity assays show that the newly designed DOX loaded AuNPs are able to kill cancer cells (A549). This synthesis demonstrates the delicate arrangement of PEI-g-PEG copolymers, aptamers, and DOX on AuNPs that are achieved by sequential amide reactions. Such aptamer-PEI-g-PEG functionalized AuNPs provide a promising platform for targeted drug delivery in cancer therapy.

In this protocol, doxorubicin-loaded AS1411-g-PEI-g-PEG modified gold nanoparticles are synthesized via three-step amide reactions. Then, doxorubicin is loaded and delivered to target cancer cells for cancer therapy.

표적 약물 전달을 위해 독소루비신으로 로드된 압타머-PEI-g-PEG 수정 금 나노 입자의 합성

Due to drug resistance and toxicity in healthy cells, use of doxorubicin (DOX) has been limited in clinical cancer therapy. This protocol describes the ...