A practical guide to quartz crystal microbalance with dissipation monitoring of thin polymer films

Easley, Alexandra D.; Ma, Ting; Eneh, Chikaodinaka I.; Yun, Jong-Won; Thakur, Ratul Mitra; Lutkenhaus, Jodie L.

doi:10.1002/pol.20210324

Cited by 116 publications

(124 citation statements)

References 89 publications

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“…Regarding QCM-D data, the low values of dissipation (see inset of Figure 2a), as well as the close superposition of the different overtone signals (see Figure S2, Supporting Information) and the rather low ΔD/Δf ratio values, are indicative of rigid, low hydrated films. [57] In particular, our system is characterized by ΔD/Δf values of ≈25 × 10 −9 Hz −1 for both steps of HS-pDNA self-assembly and hybridization with tDNA. Higher ΔD/Δf values, of 60 10 −9 Hz −1 and 72 10 −9 Hz −1 , have been reported for single strand and hybridized DNA films anchored to the QCM quartz crystal through biotin/avidin coupling.…”

Section: Monitoring Hybridization: Real Time Measurementsmentioning

confidence: 99%

“…[55,56] Soft, highly hydrated films exhibiting a viscoelastic behavior are better described by the Voigt modeling. [57] The ratio of dissipation changes to frequency changes (ΔD/Δf) can provide further insight into the rigid versus viscoelastic behavior of the film, high values of the ratio being indicative of soft viscoelastic films. [23] The synergy between SPR and QCM-D [58,23] and between SE and QCM-D [24,35,[59][60][61] measurements has already been demonstrated, and will display its broad potential also in our experiments.…”

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Spectroscopic Ellipsometry Investigation of a Sensing Functional Interface: DNA SAMs Hybridization

Pinto

Dante

Rotondi

et al. 2022

Adv Materials Inter

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monitoring of therapeutic treatments. Many sensing concepts have been proposed and tested in recent years to achieve this challenging mix. For these purposes, hybrid interfaces, where a self-assembled monolayer (SAM) with the desired biofunctionality is immobilized on an inorganic substrate, represent a versatile, popular platform for effective biosensors.The impressive development regarding the fabrication of functionalized DNA strands have promoted these kinds of molecules as building blocks for the development of sensing platforms. [1][2][3] Selective and reversible hybridization between complementary strands can be exploited to detect specific biomarkers, from nucleic acid target sequences (such as miRNA, [4] ctDNA [5] or viral sequences [6] ) to proteins, by employing protein-DNA conjugates. [7][8][9][10] Clearly, the outbreak of the COVID-19 pandemic has boosted the urgent need for highly sensitive, inexpensive and rapid selective recognition of SARS-CoV-2 sequences and spurred research on DNA-based detection of viral sequences. [11,12] In this work, we analyze a DNA sensing concept that is implemented through a 3-step process (Figure 1). The process is initiated with the self-assembly of single-strand DNA (HS-pDNA, 22 bases) that binds to gold through a linker (hexanethiol, C6). According to well-defined protocols, [13] this SAM is exposed to mercaptohexanol (MCH), a thiol with the same alkyl chain length of the hexanethiol linker. It has been reported that MCH co-adsorption improves DNA film organization [14][15][16][17] and increases the efficiency of the final, hybridization step [18,19] that implements the recognition of the target sequence.Literature presents varieties of methods for the recognition of target sequences through the formation of double-strand DNA (dsDNA). Some approaches involve mass sensitive methods like Quartz Crystal Microbalance (QCM) [20][21][22][23][24] or electrochemical methods. [25][26][27][28] Optical methods have been proposed that exploit, among others, colorimetric detection, [29] Surface Plasmon Resonance phenomena (SPR) [22,23,30] or combined plasmonic photothermal effects and localized SPR. [31] SPR, in particular, has been valuably employed to study surface confined DNA hybridization on a system closely related to the one under investigation here. [32] Among optical methods, Spectroscopic Ellipsometry (SE) can be advantageously employed to track changes in film Here, a comprehensive study of a label-free detection platform for the recognition of oligonucleotide sequences based on hybridization of thioltethered DNA strands self-assembled on flat gold films is presented. The study exploits in-buffer spectroscopic ellipsometry (SE) measurements, a noninvasive method sensitive to monolayer films, supported by surface mass density change measurements (Quartz Crystal Microbalance with Dissipation, QCM-D) obtained under comparable experimental conditions. SE and QCM-D allow monitoring deposition of molecular precursors and DNA chain hybridization. Combining SE measurements wi...

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Section: Monitoring Hybridization: Real Time Measurementsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Spectroscopic Ellipsometry Investigation of a Sensing Functional Interface: DNA SAMs Hybridization

Pinto

Dante

Rotondi

et al. 2022

Adv Materials Inter

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“…We here present a method to quantify the mean size of GAGs that are attached with one end to a planar surface. The method is based on quartz crystal microbalance with dissipation monitoring (QCM-D), a technique that is widely used for the analysis of macromolecular interactions and thin films at surfaces 38 – 40 . Through measuring changes in the resonance frequency (Δ f ) and the so-called energy dissipation (Δ D ; related to the rate of decay of the induced oscillations) of a shear-oscillating quartz crystal sensor with sub-second time resolution, QCM-D can monitor changes in the mass per unit surface area (areal mass density) indicating binding, along with the mechanical characteristics of the surface-bound film in real time.…”

Section: Introductionmentioning

confidence: 99%

A quartz crystal microbalance method to quantify the size of hyaluronan and other glycosaminoglycans on surfaces

Srimasorn

Souter

Green

et al. 2022

Sci Rep

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Hyaluronan (HA) is a major component of peri- and extra-cellular matrices and plays important roles in many biological processes such as cell adhesion, proliferation and migration. The abundance, size distribution and presentation of HA dictate its biological effects and are also useful indicators of pathologies and disease progression. Methods to assess the molecular mass of free-floating HA and other glycosaminoglycans (GAGs) are well established. In many biological and technological settings, however, GAGs are displayed on surfaces, and methods to obtain the size of surface-attached GAGs are lacking. Here, we present a method to size HA that is end-attached to surfaces. The method is based on the quartz crystal microbalance with dissipation monitoring (QCM-D) and exploits that the softness and thickness of films of grafted HA increase with HA size. These two quantities are sensitively reflected by the ratio of the dissipation shift (ΔD) and the negative frequency shift (− Δf) measured by QCM-D upon the formation of HA films. Using a series of size-defined HA preparations, ranging in size from ~ 2 kDa tetrasaccharides to ~ 1 MDa polysaccharides, we establish a monotonic yet non-linear standard curve of the ΔD/ − Δf ratio as a function of HA size, which reflects the distinct conformations adopted by grafted HA chains depending on their size and surface coverage. We demonstrate that the standard curve can be used to determine the mean size of HA, as well as other GAGs, such as chondroitin sulfate and heparan sulfate, of preparations of previously unknown size in the range from 1 to 500 kDa, with a resolution of better than 10%. For polydisperse samples, our analysis shows that the process of surface-grafting preferentially selects smaller GAG chains, and thus reduces the average size of GAGs that are immobilised on surfaces comparative to the original solution sample. Our results establish a quantitative method to size HA and other GAGs grafted on surfaces, and also highlight the importance of sizing GAGs directly on surfaces. The method should be useful for the development and quality control of GAG-based surface coatings in a wide range of research areas, from molecular interaction analysis to biomaterials coatings.

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“…We here present a method to quantify the mean size of GAGs that are attached with one end to a planar surface. The method is based on quartz crystal microbalance with dissipation monitoring (QCM-D), a technique that is widely used for the analysis of macromolecular interactions and thin films at surfaces [37][38][39]. Through measuring changes in the resonance frequency (Δf) and the energy dissipation (ΔD; the rate of decay of the induced oscillations) of a shear-oscillating quartz crystal sensor with sub-second time resolution, QCM-D can monitor changes in the mass per unit surface area (areal mass density) indicating binding, along with the mechanical characteristics of the surface-bound film in real time.…”

Section: Introductionmentioning

confidence: 99%

A quartz crystal microbalance method to quantify the size of hyaluronan and other glycosaminoglycans on surfaces

Srimasorn

Souter

Green

et al. 2022

Preprint

View full text Add to dashboard Cite

Hyaluronan (HA) is a major component of peri- and extra-cellular matrices and plays important roles in many biological processes such as cell adhesion, proliferation and migration. The abundance, size distribution and presentation of HA dictate its biological effects and are also useful indicators of pathologies and disease progression. Methods to assess the molecular mass of soluble HA and other glycosaminoglycans (GAGs) are well established. In many biological and technological settings, however, GAGs are displayed on surfaces, and methods to obtain the size of surface-attached GAGs are lacking. Here, we present a method to size HA that is end-attached to surfaces. The method is based on the quartz crystal microbalance with dissipation monitoring (QCM-D) and exploits that the softness and thickness of films of grafted HA increase with HA size. These two quantities are sensitively reflected by the ratio of the dissipation shift (ΔD) and the negative frequency shift (-Δf) measured by QCM-D upon the formation of HA films. Using a series of size-defined HA preparations, ranging in size from a tetrasaccharide to a 1 MDa polysaccharide, we establish a standard curve of the ΔD/-Δf ratio as a function of HA size. We demonstrate that the standard curve can be used to determine the mean size of HA, as well as other GAGs, such as chondroitin sulfate and heparan sulfate, of preparations of previously unknown size in the range from 1 to 500 kDa, and with a resolution better than 10%. For polydisperse samples, our analysis shows that the process of surface-grafting preferentially selects smaller GAG chains, and thus reduced the average size of GAGs that are immobilised on surfaces comparative to the original solution sample. Our results establish a quantitative method to size HA and other GAGs grafted on surfaces, and also highlight the importance of sizing GAGs directly on surfaces. The method should be useful for the development and quality control of GAG-based surface coatings in a wide range of research areas, from molecular interaction analysis to biomaterials coatings.

show abstract

A practical guide to quartz crystal microbalance with dissipation monitoring of thin polymer films

Cited by 116 publications

References 89 publications

Spectroscopic Ellipsometry Investigation of a Sensing Functional Interface: DNA SAMs Hybridization

Spectroscopic Ellipsometry Investigation of a Sensing Functional Interface: DNA SAMs Hybridization

A quartz crystal microbalance method to quantify the size of hyaluronan and other glycosaminoglycans on surfaces

A quartz crystal microbalance method to quantify the size of hyaluronan and other glycosaminoglycans on surfaces

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