Size Exclusion Chromatography: An Indispensable Tool for the Isolation of Monodisperse Gold Nanomolecules

Highly monodisperse and pure samples of atomically precise gold nanomolecules (AuNMs) are essential to understand their properties and to develop applications using them. Unfortunately, the synthetic protocols that yield a single-sized nanomolecule in a single-step reaction are unavailable. Instead,...

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Published inAnalytical chemistry (Washington) Vol. 93; no. 8; pp. 3987 - 3996
Main Authors Sakthivel, Naga Arjun, Jupally, Vijay Reddy, Eswaramoorthy, Senthil Kumar, Wijesinghe, Kalpani Hirunika, Nimmala, Praneeth Reddy, Kumara, Chanaka, Rambukwella, Milan, Jones, Tanya, Dass, Amala
Format Journal Article
LanguageEnglish
Published United States American Chemical Society 02.03.2021
Subjects
analytical chemistry
Chemistry
Chromatography
Fractionation
gel chromatography
Gold
Ions
ligands
Mass spectrometry
Mass spectroscopy
Nanoparticles
Separation
Separation techniques
Size exclusion chromatography
solubility
Solvent fractionation
Solvents
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Abstract Highly monodisperse and pure samples of atomically precise gold nanomolecules (AuNMs) are essential to understand their properties and to develop applications using them. Unfortunately, the synthetic protocols that yield a single-sized nanomolecule in a single-step reaction are unavailable. Instead, we observe a polydisperse product with a mixture of core sizes. This product requires post-synthetic reactions and separation techniques to isolate pure nanomolecules. Solvent fractionation based on the varying solubility of different sizes serves well to a certain extent in isolating pure compounds. It becomes tedious and offers less control while separating AuNMs that are very similar in size. Here, we report the versatile and the indispensable nature of using size exclusion chromatography (SEC) as a tool for separating nanomolecules and nanoparticles. We have demonstrated the following: (1) the ease of separation offered by SEC over solvent fractionation; (2) the separation of a wider size range (∼5–200 kDa or ∼1–3 nm) and larger-scale separation (20–100 mg per load); (3) the separation of closely sized AuNMs, demonstrated by purifying Au137(SR)56 from a mixture of Au329(SR)84, Au144(SR)60, Au137(SR)56, and Au130(SR)50, which could not be achieved using solvent fractionation; (4) the separation of AuNMs protected by different thiolate ligands (aliphatic, aromatic, and bulky); and (5) the separation can be improved by increasing the column length. Mass spectrometry was used for analyzing the SEC fractions.
AbstractList Highly monodisperse and pure samples of atomically precise gold nanomolecules (AuNMs) are essential to understand their properties and to develop applications using them. Unfortunately, the synthetic protocols that yield a single-sized nanomolecule in a single-step reaction are unavailable. Instead, we observe a polydisperse product with a mixture of core sizes. This product requires post-synthetic reactions and separation techniques to isolate pure nanomolecules. Solvent fractionation based on the varying solubility of different sizes serves well to a certain extent in isolating pure compounds. It becomes tedious and offers less control while separating AuNMs that are very similar in size. Here, we report the versatile and the indispensable nature of using size exclusion chromatography (SEC) as a tool for separating nanomolecules and nanoparticles. We have demonstrated the following: (1) the ease of separation offered by SEC over solvent fractionation; (2) the separation of a wider size range (∼5–200 kDa or ∼1–3 nm) and larger-scale separation (20–100 mg per load); (3) the separation of closely sized AuNMs, demonstrated by purifying Au₁₃₇(SR)₅₆ from a mixture of Au₃₂₉(SR)₈₄, Au₁₄₄(SR)₆₀, Au₁₃₇(SR)₅₆, and Au₁₃₀(SR)₅₀, which could not be achieved using solvent fractionation; (4) the separation of AuNMs protected by different thiolate ligands (aliphatic, aromatic, and bulky); and (5) the separation can be improved by increasing the column length. Mass spectrometry was used for analyzing the SEC fractions.
Highly monodisperse and pure samples of atomically precise gold nanomolecules (AuNMs) are essential to understand their properties and to develop applications using them. Unfortunately, the synthetic protocols that yield a single-sized nanomolecule in a single-step reaction are unavailable. Instead, we observe a polydisperse product with a mixture of core sizes. This product requires post-synthetic reactions and separation techniques to isolate pure nanomolecules. Solvent fractionation based on the varying solubility of different sizes serves well to a certain extent in isolating pure compounds. It becomes tedious and offers less control while separating AuNMs that are very similar in size. Here, we report the versatile and the indispensable nature of using size exclusion chromatography (SEC) as a tool for separating nanomolecules and nanoparticles. We have demonstrated the following: (1) the ease of separation offered by SEC over solvent fractionation; (2) the separation of a wider size range (∼5–200 kDa or ∼1–3 nm) and larger-scale separation (20–100 mg per load); (3) the separation of closely sized AuNMs, demonstrated by purifying Au137(SR)56 from a mixture of Au329(SR)84, Au144(SR)60, Au137(SR)56, and Au130(SR)50, which could not be achieved using solvent fractionation; (4) the separation of AuNMs protected by different thiolate ligands (aliphatic, aromatic, and bulky); and (5) the separation can be improved by increasing the column length. Mass spectrometry was used for analyzing the SEC fractions.
Highly monodisperse and pure samples of atomically precise gold nanomolecules (AuNMs) are essential to understand their properties and to develop applications using them. Unfortunately, the synthetic protocols that yield a single-sized nanomolecule in a single-step reaction are unavailable. Instead, we observe a polydisperse product with a mixture of core sizes. This product requires post-synthetic reactions and separation techniques to isolate pure nanomolecules. Solvent fractionation based on the varying solubility of different sizes serves well to a certain extent in isolating pure compounds. It becomes tedious and offers less control while separating AuNMs that are very similar in size. Here, we report the versatile and the indispensable nature of using size exclusion chromatography (SEC) as a tool for separating nanomolecules and nanoparticles. We have demonstrated the following: (1) the ease of separation offered by SEC over solvent fractionation; (2) the separation of a wider size range (∼5-200 kDa or ∼1-3 nm) and larger-scale separation (20-100 mg per load); (3) the separation of closely sized AuNMs, demonstrated by purifying Au137(SR)56 from a mixture of Au329(SR)84, Au144(SR)60, Au137(SR)56, and Au130(SR)50, which could not be achieved using solvent fractionation; (4) the separation of AuNMs protected by different thiolate ligands (aliphatic, aromatic, and bulky); and (5) the separation can be improved by increasing the column length. Mass spectrometry was used for analyzing the SEC fractions.Highly monodisperse and pure samples of atomically precise gold nanomolecules (AuNMs) are essential to understand their properties and to develop applications using them. Unfortunately, the synthetic protocols that yield a single-sized nanomolecule in a single-step reaction are unavailable. Instead, we observe a polydisperse product with a mixture of core sizes. This product requires post-synthetic reactions and separation techniques to isolate pure nanomolecules. Solvent fractionation based on the varying solubility of different sizes serves well to a certain extent in isolating pure compounds. It becomes tedious and offers less control while separating AuNMs that are very similar in size. Here, we report the versatile and the indispensable nature of using size exclusion chromatography (SEC) as a tool for separating nanomolecules and nanoparticles. We have demonstrated the following: (1) the ease of separation offered by SEC over solvent fractionation; (2) the separation of a wider size range (∼5-200 kDa or ∼1-3 nm) and larger-scale separation (20-100 mg per load); (3) the separation of closely sized AuNMs, demonstrated by purifying Au137(SR)56 from a mixture of Au329(SR)84, Au144(SR)60, Au137(SR)56, and Au130(SR)50, which could not be achieved using solvent fractionation; (4) the separation of AuNMs protected by different thiolate ligands (aliphatic, aromatic, and bulky); and (5) the separation can be improved by increasing the column length. Mass spectrometry was used for analyzing the SEC fractions.
Highly monodisperse and pure samples of atomically precise gold nanomolecules (AuNMs) are essential to understand their properties and to develop applications using them. Unfortunately, the synthetic protocols that yield a single-sized nanomolecule in a single-step reaction are unavailable. Instead, we observe a polydisperse product with a mixture of core sizes. This product requires post-synthetic reactions and separation techniques to isolate pure nanomolecules. Solvent fractionation based on the varying solubility of different sizes serves well to a certain extent in isolating pure compounds. It becomes tedious and offers less control while separating AuNMs that are very similar in size. Here, we report the versatile and the indispensable nature of using size exclusion chromatography (SEC) as a tool for separating nanomolecules and nanoparticles. We have demonstrated the following: (1) the offered by SEC over solvent fractionation; (2) the separation of a (∼5-200 kDa or ∼1-3 nm) and separation (20-100 mg per load); (3) the separation of , demonstrated by purifying Au (SR) from a mixture of Au (SR) , Au (SR) , Au (SR) , and Au (SR) , which could not be achieved using solvent fractionation; (4) the separation of (aliphatic, aromatic, and bulky); and (5) the separation can be improved by increasing the column length. Mass spectrometry was used for analyzing the SEC fractions.
Author Nimmala, Praneeth Reddy
Kumara, Chanaka
Dass, Amala
Rambukwella, Milan
Sakthivel, Naga Arjun
Wijesinghe, Kalpani Hirunika
Eswaramoorthy, Senthil Kumar
Jones, Tanya
Jupally, Vijay Reddy
AuthorAffiliation Department of Chemistry and Biochemistry
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  orcidid: 0000-0001-6942-5451
  surname: Dass
  fullname: Dass, Amala
  email: amal@olemiss.edu
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Snippet Highly monodisperse and pure samples of atomically precise gold nanomolecules (AuNMs) are essential to understand their properties and to develop applications...
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SubjectTerms analytical chemistry
Chemistry
Chromatography
Fractionation
gel chromatography
Gold
Ions
ligands
Mass spectrometry
Mass spectroscopy
Nanoparticles
Separation
Separation techniques
Size exclusion chromatography
solubility
Solvent fractionation
Solvents
Title Size Exclusion Chromatography: An Indispensable Tool for the Isolation of Monodisperse Gold Nanomolecules
URI http://dx.doi.org/10.1021/acs.analchem.0c04961
https://www.ncbi.nlm.nih.gov/pubmed/33606508
https://www.proquest.com/docview/2498421544
https://www.proquest.com/docview/2491939325
https://www.proquest.com/docview/2524245092
Volume 93
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