Technologies
Abstract
SPE and LC
are techniques used in analysis of chemical substances that involve a
stationary phase and mobile phase. The most commonly used and universally
accepted stationary phases are based on porous silica particles. Silica based
stationary phases have the benefit of good mechanical strength, high surface
area, and strong absorption. However, they suffer from several shortcomings,
including limited pH stability, low maximum operating temperature, and wide
selectivity variation. FIU
scientists have developed a new class of
SPE sorbents and LC stationary phases using microcrystalline cellulose
particles as the substrate and sol-gel sorbent coating technology as the
polymer/sorbent immobilization technology. This invention
allows higher temperatures to be used, which is important to reduce analysis
time, enhance column efficiency, and improve detection sensitivity.
Additionally, the stationary phase support will not dissolve at high or low pH
values or temperatures.Benefit
Reduction of analysis time in chromatography Enhancement of column efficiency when performing column chromatographyImprovement of detection sensitivityHigh thermal stability (up to 350 °C)High pH stability (1-13)Market Application
Identification of components of substances in forensicsQuality assurance in the food industryIdentification and separation of contaminants
Abstract
The microextraction capsule (MEC) is capable of extracting target analyte(s)
directly from unaltered sample matrices of biological, chemical, environmental,
food, pharmaceutical, toxicological, and forensic significance containing high
volume of matrix interferents without requiring any sample clean-up approaches
prior to the extraction of the target analyte(s). Due to the high loading of
the extraction sorbent, MEC is capable of handling direct extraction from a
broad range of concentrations of the analyte(s). The sponge-like porous
architecture of the sol-gel hybrid inorganic-organic sorbents used in MEC
results in the achievement of very fast extraction equilibrium. MEC utilizes a
porous membrane to enclose sol-gel derived high efficiency extraction sorbents
that works as a filter to safeguard the integrity of the sorbent and to
permeate the aqueous solution through it for rapid sorbent-analyte interaction. The porous membrane also houses a small magnet in order to rotate the device at
a set speed under the magnetic field and significantly enhances the mass
transfer kinetic between the sample and the micro extraction capsule. The
elution process of extracted analytes can be carried out by exposing the MEC to
high temperatures in a thermal desorption unit followed by purging the released
analytes into the gas chromatography inlet by carrier gas flow or by exposing
the MEC to a small volume of organic solvent to back-extract the analyte which
can be injected into gas chromatography or liquid chromatography for detection
and quantification.Benefit
Integrates the advanced material properties of sol-gel inorganic/hybrid organic-inorganic polymeric networks offering (i) adjustable porosity; (ii) tunable selectivity; (iii) high thermal and solvent stability; (iv) wide range of pH stability (1-13)Provides a tubular porous membrane capable of retaining and protecting the extraction sorbent while keeping it accessible to the aqueous solution containing the analytes of interestPromotes faster analyte mass transfer by providing a magnetic stirring mechanism resulting in a standalone solvent minimized or solvent-less micro extraction device which provides near exhaustive extraction even under equilibrium extraction conditionsMarket Application
This technology is capable of performing efficient extraction and pre-concentration of organic analytes, cations, anions and heavy metals from a variety of sources including:Forensic specimens such as blood, urine, plasma, serum, saliva.Pollutants from environment waterChemical and pharmaceutical samplesDrug or poison residues from biological samplesFood samplesPublications
Samanidou, V., Georgiadis, D., Kabir, A., Furton, K., Capsule phase microextraction:
the total and ultimate sample preparation approach. J. Chromatogr. Sep. Tech. 2018, 9, 1– 4.
Abstract
Currently available bonded phases
used in HPLC, UPLC and SPE employ silica particles as the base material. To
increase the phases applicability and adaptability, the surface of the
particles can further be modified by bonding a wide variety of functional groups
to the surface: non-polar (e.g. C18), polar (e.g. NH2), ionic (e.g.
propylsulphonic acid) or mixed-mode (e.g. C8/cation exchange). However, the state-of-the-art
approach to preparing bonded silica particles results in a number of inherent
shortcomings. For example, a thin coating of the bonded phase must provide all
of the required analyte/sorbent/stationary phase interactions, which imposes a
requirement of a high volume of stationary phase loaded into a long column size
to achieve a large sample breakthrough volume, which is the maximum sample
volume that can be passed through the column without saturating the bed with
the analytes. Often there is an insufficient organic group loading per unit
mass of the stationary phase/SPE sorbent to achieve adequate separation or
absorption. Finally, the state-of-the-art
phases display a very narrow range of pH stability, typically, at best, having
a robust stationary phase when maintained within a pH range of 2 to 8.FIU inventors have developed
sol-gel synthesis of alkyl functionalized (e.g., C4, C8, C12, C18) HPLC, UPLC and SPE sorbents. The synthetic method employs a tetrafunctional
silane and a trifunctional silane containing a sorbent functionality, for
example, tetraalkoxy silane and an alkyltrialkoxy silane or their equivalents
in presence of either an acid catalyst, an acid catalyst followed by a base
catalyst, or a base catalyst. This method yields a chemically and structurally
more stable highly porous hybrid inorganic-inorganic material. Due to the high
porosity and extremely high surface area, the HPLC stationary phase and SPE
sorbents offer more analyte-alkyl functional group interactions per unit mass
of the stationary phases/SPE sorbents, consequently minimizing the required
mass of the stationary phases/SPE sorbents to achieve target chromatographic
separation and extraction efficiency. Additionally, consumption of organic
solvents in chromatographic separation and sample preparation is significantly
reduced.Benefit
Eliminates the use of preformed silica particles as the inert surface to graft different alkyl pendant groups via silane surface modificationDisplays high porosity and high surface areaOffers high chromatographic selectivity, separation power, and extraction efficiencyDisplays high thermal, chemical and solvent stability, as well as extended pH stability (pH 1-12)Requires less volume of solvent during chromatographic separation or SPE elutionEliminates solvent evaporation and sample reconstitution when used as SPE sorbentsMarket Application
HPLC stationary phases in both convention columns (5 micrometer particle size)UHPLC columns (submicron particle size)SPE reverse phase sorbents
Abstract
Dynamic Fabric Phase Sorptive Extraction (DFPSE) disks are capable of extracting target analyte(s)
exhaustively from unmodified sample matrices containing high volume of matrix
interferents including particles, debris, biomass, cells, tissues, proteins
without employing any sample clean-up exercise.The technology
provides the process of making DFPSE disks by chemically immobilizing organic
polymers or ligands on a flexible substrate resulting in an exhaustive sample
preparation (cleaning/preconcentration) to accomplish high recovery of target
analyte(s) in a short period of time.DFPSE provides
flexible, open, flat and easily accessible surface for rapid sorbent-analyte
interaction. Since both the surfaces and inner matrix of the substrate are
coated with inherently porous sol-gel hybrid materials, the accessible surface
area for DFPSE media are enormous leading to a very high sample capacity.In DFPSE, any organic
solvent or solvent mixture can be used as the eluent/back-extraction solvent
since the composite coatings are chemically bonded to the substrate. As a
result, same sample can be analyzed in GC/HPLC/CE if a mutually compatible
solvent is chosen for the back-extraction. Utilization of proper solvent for
back-extraction also ensures no analyte carry-over that may hinders future
extractions or compromises the quality of analytical data. Also, high
enrichment factors obtained in DFPSE eliminates the necessity of time consuming
solvent evaporation and sample reconstitution step.Due to the strong
covalent bonding between the hybrid coating and the substrate, the coating
demonstrates high chemical stability and can be exposed to high acidic (pH 1)
and basic (pH 12) environment without compromising the integrity of the
extraction disk.DFPSE allows user to
use disks coated with polymers of different polarity. As a result, if the
objective of the analytical scheme is to extract analytes with different
polarity, multiple disks coated with different polarity can be employed. At the
end, all extracted analytes can be back-extracted in the same back-extraction
solvent.Benefit
Fast and highly sensitive sampling and sample preparation capabilityFlexible, highly reproducible, portable and easy to useVery high sample capacity translates into high break-through volumeHigh chemical and solvent stability allows exposure to any organic solvent and aqueous solution with pH ranges of 1-12Market Application
Collection and preconcentration of target analytes from unmodified sample matrix of chemical, biochemical, pharmaceutical, forensic, clinical, and environmental significance
Abstract
Sample preparation is an integral
and perhaps the most important step in chemical analysis. However, current
techniques employed for preparing samples are multi-step, laborious, expensive,
and often unreliable. Therefore, a need remains for solvent free or solvent
minimized microextraction devices that permit the acquisition of low
concentrations of analytes present in a wide range of aqueous or other liquid
environments.FIU inventors have developed
in-vial microextraction (IVME) method and IVME devices that are sample
collection vials. These vials have a sorbent coating on at least a portion of
the inner surface of the vial, and a sorbent coating of the same of different composition
on at least a portion of the outer surface of the vial. The sorbent coating are
constructed on the surface of the vial using sol-gel coating technology, and
comprise metal oxide comprising gels that are capable of absorbing at least one
target analyte. These vials can be of different size, shape, and construction
materials.Benefit
Enables both sampling and sample preparation in the field Permits the acquisition of low concentrations of analytes present in a wide range of aqueous or other liquid environments Can be used by untrained individuals to provide truly representative sample Allows the work up of the samples in a simple and effective mannerMarket Application
Sample preparation for a wide variety of analytes in various fields such as biological, environmental, clinical, toxicological, food, pharmaceutical, bio-analytical, and forensic.
Abstract
This method has proved to be effective in obtaining humans profiles demonstrating humans scent variability which can serve as a potential human identification/detection tool in forensics and as a technique to monitor odor changes cause by the onset of a disease in the medical field. Up to recently there were technology limitations to differentiate individuals based on their odor; one of the most common tools was the use of trained canine, therefore this novel invention can create a new field in human identification as a biometric measurement. The scarcity of scientific background pertaining to human odor and scent collection methods has led to successful legal challenges to the use of canine human scent discriminations for investigative purposes; this invention could address this issue in the criminal justice field. The technique developed by FIU researchers could also impact the medical field as it can establish the base odor of an individual and monitor the change in such individual’s odor due to a disease. This technique could represent a new diagnostic tool that can easily alert to the potential onset of a disease just by one’s scent. Benefit
Rapid and reliableCost effectiveMinimum sample is requiredHighly specific and sensitiveMarket Application
Compounds of the human scent can be used in forensic field as an identification tool and in security at port of entriesThe technology is also applicable in the medical field and for genetic research
Abstract
Biological detector animals, such
as canines, are valuable tools for the rapid, onsite detection of illicit
materials; however, they require extensive training to ensure field
deployability with high degree of reliability. A safe method of training
involves the uses of mimics, in which biological detector animals are presented
with the active odors of volatile organic compounds that mimic the odors of the
contraband they are being trained on.Currently available training aids
suffer from very specific drawbacks, including short shelf life, field
contamination concerns, and limited dissipation manipulation capabilities.Researchers at FIU have developed
a training aid that allows handlers to adjust the abundance of odors presented
to their animals, familiarizing themselves with their animal’s strengths and
weaknesses. Dissipation rate can also be controlled through temperature
adjustments. Most importantly, the training aids have the unique ability of not
dissipating any odors when frozen. This is particularly advantageous because it
allows for preservation of the training materials when being shipped or stored.Benefit
Provides six times longer shelf-life than currently available training aids Allows for polymeric network manipulation, temperature manipulation, and polymer containment Is significantly less prone to field contamination Is a cost efficient option for animal handlers and trainersMarket Application
Drug and/or explosive animal training facilities such as K-9 unit, and TSA
Abstract
Detection of ultra-trace level of
contaminants in complex food, biological and/or environmental samples is often
necessary for health and safety reasons. Unfortunately, such detection is often
difficult, due to a variety of reasons, including the complexity of the samples
that are being tested, and the presence of numerous potential interferents in
these samples. MIPs are synthetic polymeric materials that possess specific
cavities complimentary to the shape, size, and functional groups of a template molecule
used in the imprinting process. Currently, several techniques exist for the
synthesis of MIPs; however, they suffer from several drawbacks such as
non-specific adsorption, low adsorption capacity, low imprinting factor, low
sample throughput, and irreversible analyte loss leading to ineffective removal
of the template and poor data quality.FIU inventors have developed
chemical compositions and synthesis strategies to create MIPs via sol-gel processes
using organic, inorganic, or metallic target analyte. The resulting MIPs are
hybrid organic-inorganic or inorganic three-dimensional network exhibiting high
affinity towards a target analyte and its structural analogs and remain
indifferent to other molecules or species present in the same sample matrix.Benefit
Offers an effective strategy to create MIPs having high affinity towards the analyte(s) of interest, similar to antibody-antigen interactions Provides substrates with adjustable porosity, tunable selectivity, high thermal stability, solvent stability, and stability over a wide range of pHMarket Application
Detection and extraction of small amounts of substances in food, biological and environmental samples Controlled release drug deliveryPublications
Kechagia M, Samanidou V, Kabir A,
Furton KG. One-pot synthesis of a multi-template molecularly imprinted polymer
for the extraction of six sulfonamide residues from milk before
high-performance liquid chromatography with diode array detection. J Sep Sci.
2018;41(3):723-731. doi:10.1002/jssc.201701205
Biosciences
Abstract
Supports for reversed phase high-performance liquid
chromatography (RP-HPLC) column, normal phase high-performance liquid
chromatography (NP-HPLC) column, and hydrophilic interaction liquid
chromatography (HILIC) column are silica particles coated with organic ligands
via silane chemistry. As a result, only a very small portion of the stationary
phase contributes to retention and selectivity. The currently used bonded
phases for these chromatography columns suffer from a number of shortcomings:
silica particles limit the loading of organic ligands, which leaves many
surface silanol groups unattended on the silica surface, and results in
chemical instability, particularly when using basic solvents. FIU inventors have developed sol-gel sorbent or
chromatography stationary phase comprising particles of a metal oxide gel
containing polymeric segments uniformly distributed throughout the metal oxide
gel. The chemical incorporation of various organic polymers into the sol-gel
hybrid inorganic-organic matrix opens up the possibility of creating hundreds
of novel sorbents with unique selectivity.Benefit
Eliminates the need of using silica substrate to hold different polar functional moietiesDisplays high resistance against high temperature, harsh chemical environment, with pH stability that can range from 1-13Provides a high surface area for rapid interaction with the analyte(s).Eliminates the need of solvent evaporation and sample reconstitution when used as SPE sorbentsMarket Application
Food, pharmaceutical, environmental, toxicological, clinical, and forensic analysisEnvironmental remediation and antimicrobial and/or other protective coatings in food or pharmaceutical packaging
Abstract
Traditionally, a large number
of particulate matters are used individually or in different combination as
adsorbents in water filtration system, air pollutant trapping systems, sewage
treatments plants, to name a few. Many of these particulate matters possess
extremely high surface area, but disadvantageously demonstrate a strong
tendency to form agglomeration, therefore excluding a large portion of these
particles' available surface area to analytes. FIU inventors have developed carbonaceous and
non-carbonaceous particulate matters encapsulated in sol-gel sorbent matrices,
and methods of synthesizing them. The addition of particulate matters in the
sol solution during sol-gel synthesis results in a sol-gel composite sorbent
system with homogeneously trapped particulate matters in a permeable cage-like
architecture. Due to the inherently porous and open architecture of a sol-gel
silica network, encapsulated particulate matters maintain high surface area and
freely accessible interaction sites. The unique combination of the particulates
into sol-gel matrix synergistically augments the material properties of the composite
material system to offer unique selectivity and affinity towards most of the
target analytes. These analytes include emerging pollutants, EPA priority
pollutants, heavy metals ionic and ionizable compounds, endocrine disrupting
chemicals, and other pollutants and unwanted entities in water and air.Benefit
Possess high porosity, high surface area, and high thermal and chemical stabilityProvide superior chromatographic selectivity and excellent extraction efficiencyCan be used for a wide range of analytes including polar, medium polar, nonpolar, ionic, and metal speciesMarket Application
These sol-gel encapsulated particulate matters can be employed in water filtration, environmental pollution remediation, wastewater treatment, air pollution monitoring and mitigation, as well as sorbents in solid phase extraction and solid phase microextraction.
Abstract
Poly(ethylene glycol) is commonly
used as a polar polymer for immobilization on a substrate’s surface. However,
immobilization of polar polymers, including PEG, on a substrate’s surface is
still considered a challenge to surface chemists. The resulting substrates
often display long extraction time, low solvent resistance, and low thermal
stability. In addition, even though the incorporation of PEG polymer in the
sol-gel matrix (sol-gel coating technology) improves solvent resistance and
thermal stability of the composite material, the limited polarity of PEG
remains a problem when employed to target highly polar analytes.FIU inventors have designed and
synthesized highly polar chromatographic stationary phases and adsorption
sorbents comprising a sol-gel network of metal(s) oxide precursor condensed
with highly polar polyhydroxy molecule(s). This synthesis offers a simple and
environmental friendly approach of immobilization of highly polar molecules to
a metal oxide network for use as superpolar stationary phase and/or extraction
sorbent. The resulting superpolar sorbent networks can have properties derived
from being a sol-gel inorganic/hybrid organic-inorganic polymeric network that
can be formulated to display adjustable porosity, tunable selectivity, high
thermal stability, solvent stability, and wide pH stability.Benefit
Provides highly polar chromatographic stationary phases and adsorption sorbents for solid phase extraction or solid phase microextraction that can be effectively applied for polar, medium polar, nonpolar, and polarizable analytesProvides substrate with adjustable porosity, tunable selectivity, high thermal stability, solvent stability, and a wide range of pH stabilityOffers a simple, highly reproducible, and environmentally friendly synthesisMarket Application
Can be an element of a sampling device, for example an extraction device such as a fiber superpolar microextraction fiber, superpolar microextraction tube, superpolar microextraction membrane, superpolar microextraction stir bar, superpolar microextraction fabric, superpolar microextraction capsule, or superpolar microextraction vial, or solid phase extractor selected from a matrix solid phase dispersant, a magnetic solid phase extractor, or a dynamic fabric phase sorptive extractorCan be a component of an analytical device such as gas chromatograph, and liquid chromatograph stationary phase
Abstract
FIU inventors created a media for sampling and sample preparation for the analysis of trace and ultra-trace level of organic analytes that can be applied to different sample matrices of interest. The media utilizes a sol-gel process to create a hybrid organic-inorganic polymeric network and to anchor the polymeric network onto the surface of flexible substrate materials. The chemically bonded sorbent system offers very high specific surface area, and excellent chemical and high thermal stability. The media has been successfully tested in solvent minimized or solvent-less microextraction conditions for the extraction of trace and ultra-trace levels of organic analytes including highly polar analytes from different sample matrices. Sample preparation with this media is equally compatible with gas chromatography, liquid chromatography, capillary electrophoresis and other analytical instruments. Hence, the FPSE provides an improved new generation technique for trace and ultra-trace sample preparation for instrumental analysis. We are looking for a business partner to further develop and commercialize the Novel FPSE as a viable alternative to commercially available techniques and to exploit its scientific and business potential as a highly sensitive sampling and sample preparation media for trace and ultra-trace analytes from different matrices including biological, environmental, chemical, forensic, toxicological, and pharmaceutical importance. Benefit
Allows sampling and sample preparation for trace and ultra-trace level concentration of analytes from different matrices without matrix modification or pre-treatmentProvides the flexibility for sampling, storage, transport and testing in different environments as it can be used in extended form or draped around a surfacePromotes specificity for sampling of various analytes due to availability of a wide range of sorbent chemistries to provide specific interaction(s) toward the target analyte/compound classOffers part per quadrillion (ppq) level sensitivity for both polar and medium polar analytesMarket Application
Sampling and sample preparation of analytes with forensics, toxicological, national security, public health, environmental, food, bio-analytical, clinical and pharmaceutical significancePublications
Fabric Phase Sorptive Extraction in
Pharmaceutical Analysis; Pharmaceutica Analytica Acta 6(7):1-3; DOI: 10.4172/21532435.1000e177
Abstract
The microextraction capsule (MEC) is capable of extracting target analyte(s)
directly from unaltered sample matrices of biological, chemical, environmental,
food, pharmaceutical, toxicological, and forensic significance containing high
volume of matrix interferents without requiring any sample clean-up approaches
prior to the extraction of the target analyte(s). Due to the high loading of
the extraction sorbent, MEC is capable of handling direct extraction from a
broad range of concentrations of the analyte(s). The sponge-like porous
architecture of the sol-gel hybrid inorganic-organic sorbents used in MEC
results in the achievement of very fast extraction equilibrium. MEC utilizes a
porous membrane to enclose sol-gel derived high efficiency extraction sorbents
that works as a filter to safeguard the integrity of the sorbent and to
permeate the aqueous solution through it for rapid sorbent-analyte interaction. The porous membrane also houses a small magnet in order to rotate the device at
a set speed under the magnetic field and significantly enhances the mass
transfer kinetic between the sample and the micro extraction capsule. The
elution process of extracted analytes can be carried out by exposing the MEC to
high temperatures in a thermal desorption unit followed by purging the released
analytes into the gas chromatography inlet by carrier gas flow or by exposing
the MEC to a small volume of organic solvent to back-extract the analyte which
can be injected into gas chromatography or liquid chromatography for detection
and quantification.Benefit
Integrates the advanced material properties of sol-gel inorganic/hybrid organic-inorganic polymeric networks offering (i) adjustable porosity; (ii) tunable selectivity; (iii) high thermal and solvent stability; (iv) wide range of pH stability (1-13)Provides a tubular porous membrane capable of retaining and protecting the extraction sorbent while keeping it accessible to the aqueous solution containing the analytes of interestPromotes faster analyte mass transfer by providing a magnetic stirring mechanism resulting in a standalone solvent minimized or solvent-less micro extraction device which provides near exhaustive extraction even under equilibrium extraction conditionsMarket Application
This technology is capable of performing efficient extraction and pre-concentration of organic analytes, cations, anions and heavy metals from a variety of sources including:Forensic specimens such as blood, urine, plasma, serum, saliva.Pollutants from environment waterChemical and pharmaceutical samplesDrug or poison residues from biological samplesFood samplesPublications
Samanidou, V., Georgiadis, D., Kabir, A., Furton, K., Capsule phase microextraction:
the total and ultimate sample preparation approach. J. Chromatogr. Sep. Tech. 2018, 9, 1– 4.