Direct Coupling of Dispersive Extractions with Magnetic Particles to Mass Spectrometry via Microfluidic Open Interface

Microextraction coupled to mass spectrometry (MS) has great potential in analytical chemistry laboratories operating in a variety of fields. Indeed, microextraction methods directly coupled to MS can be of large value given that they can provide not only analyte extraction and enrichment but also effective sample cleanup. In recent years, the practicality in handling high active surface area, versatility, and environmentally friendly features of magnetic dispersive microextraction technologies has contributed to an explosion in the number of methods and technologies reported in the literature for a wide range of applications. However, to the best of our knowledge, no technology to date has been capable of efficiently merging these two rising concepts in a simple and integrated analytical workflow. In this context, the microfluidic open interface is presented for the direct coupling of dispersive magnetic extraction to mass spectrometry. This technology operates under the concept of a flow-isolated desorption volume, which generates a stagnant droplet open to ambient conditions while continuously feeding the ionization source with solvent by means of the self-aspiration process intrinsic of the electrospray ionization (ESI) interface. To improve the efficiency of the final analytical workflow, a novel dispersive magnetic micro- and nanoparticle extraction protocol for biofluid droplets was developed. The final methodology entailed the dispersion of a small amount of magnetic particles (20-70 μg) in a droplet of biofluid (≤40 μL) for extraction, followed by a particle collection step using a homemade 3D-printed holder containing an embedded rare-earth magnet. In the final step, the holder is set on top of the microfluidic open interface (MOI) for desorption in the isolated droplet. Switching the valve transfers the desorbed analytes to the ESI source in less than 5 s. As proof of concept, the completely new setup was applied to the determination of prohibited substances from phosphate-buffered saline (PBS) and human urine using Fe 2 O 3 magnetic nanoparticles (50 nm) functionalized with C 18 . The limits of quantitation (LOQs) obtained were in the low-ppb range in all cases, and acceptable precision (≤20%) and accuracy (80-120%) were attained. Also, taking advantage of the fast extraction kinetics provided by the radial diffusion associated with small particles, we employed the methodology for the selective extraction of phosphopeptides from 40 μL of tryptic β-casein digest using 70 μg of magnetic Ti-IMAC microparticles. To conclude, the technology and methodology herein presented provided excellent capabilities comparable to those of other solid-phase microextraction (SPME-MS) approaches while dramatically minimizing the amount of sample and sorbent required per analysis, as well as affording significantly fast extraction times due to the enhanced kinetics of extraction.Fil: Tascon, Marcos. University of Waterloo; Canadá. Universidad Nacional de San Martín. Instituto de Investigación e Ingeniería Ambiental. - Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Instituto de Investigación e Ingeniería Ambiental; ArgentinaFil: Singh, Varoon. University of Waterloo; CanadáFil: Huq, Mohammad. University of Waterloo; CanadáFil: Pawliszyn, Janusz. University of Waterloo; Canad

Direct Coupling of Dispersive Extractions with Magnetic Particles to Mass Spectrometry via Microfluidic Open Interface

Microextraction coupled to mass spectrometry (MS) has great potential in analytical chemistry laboratories operating in a variety of fields. Indeed, microextraction methods directly coupled to MS can be of large value given that they can provide not only analyte extraction and enrichment but also effective sample cleanup. In recent years, the practicality in handling high active surface area, versatility, and environmentally friendly features of magnetic dispersive microextraction technologies has contributed to an explosion in the number of methods and technologies reported in the literature for a wide range of applications. However, to the best of our knowledge, no technology to date has been capable of efficiently merging these two rising concepts in a simple and integrated analytical workflow. In this context, the microfluidic open interface is presented for the direct coupling of dispersive magnetic extraction to mass spectrometry. This technology operates under the concept of a flow-isolated desorption volume, which generates a stagnant droplet open to ambient conditions while continuously feeding the ionization source with solvent by means of the self-aspiration process intrinsic of the electrospray ionization (ESI) interface. To improve the efficiency of the final analytical workflow, a novel dispersive magnetic micro- and nanoparticle extraction protocol for biofluid droplets was developed. The final methodology entailed the dispersion of a small amount of magnetic particles (20-70 μg) in a droplet of biofluid (≤40 μL) for extraction, followed by a particle collection step using a homemade 3D-printed holder containing an embedded rare-earth magnet. In the final step, the holder is set on top of the microfluidic open interface (MOI) for desorption in the isolated droplet. Switching the valve transfers the desorbed analytes to the ESI source in less than 5 s. As proof of concept, the completely new setup was applied to the determination of prohibited substances from phosphate-buffered saline (PBS) and human urine using Fe 2 O 3 magnetic nanoparticles (50 nm) functionalized with C 18 . The limits of quantitation (LOQs) obtained were in the low-ppb range in all cases, and acceptable precision (≤20%) and accuracy (80-120%) were attained. Also, taking advantage of the fast extraction kinetics provided by the radial diffusion associated with small particles, we employed the methodology for the selective extraction of phosphopeptides from 40 μL of tryptic β-casein digest using 70 μg of magnetic Ti-IMAC microparticles. To conclude, the technology and methodology herein presented provided excellent capabilities comparable to those of other solid-phase microextraction (SPME-MS) approaches while dramatically minimizing the amount of sample and sorbent required per analysis, as well as affording significantly fast extraction times due to the enhanced kinetics of extraction.Fil: Tascon, Marcos. University of Waterloo; Canadá. Universidad Nacional de San Martín. Instituto de Investigación e Ingeniería Ambiental. - Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Instituto de Investigación e Ingeniería Ambiental; ArgentinaFil: Singh, Varoon. University of Waterloo; CanadáFil: Huq, Mohammad. University of Waterloo; CanadáFil: Pawliszyn, Janusz. University of Waterloo; Canad

Development of a background electrolyte for the determination of inorganic cations in high ionic strength samples by capillary electrophoresis with indirect UV-absorption detection

In this study, a background electrolyte capable to separate and quantify inorganic cations in high ionic strength samples by UV-absorption indirect detection was designed. In this regard, the four most abundant monovalent and divalent cations in earth crust (K+ , Na+ , Ca+2, Mg+2) were selected as model compounds. A group of small carboxylic acids and, several toluidines and pyridines were evaluated as mild strength complexing agents and chromophoric probes, respectively. The optimized background electrolyte was composed of 200 mM 2,4,6-trimethylpyridine as the chromophoric probe, 250 mM lactic acid as the weak complexing agent and pH buffering reagent (adjusted to pH 4.5), and 5 % v/v methanol as organic solvent modifier. Based on a minimum number of components, it provided outstanding separation performance in less than 4 min in a wide linear dynamic range (10 - 2500 µg∙mL-1 ). Performances were contrasted against a reference method based on conductometric detection. Furthermore, studies of separation efficiency and peak shape were carried out at different analyte concentrations in high electric conductivity solutions. The herein developed method demonstrated exceptional features in terms of limits of detection (~10 µg∙mL-1 ), resolution, speed of analysis, sensitivity and peak capacity in high electric conductivity samples. Moreover, the method was successfully applied to high ionic strength samples such as rock digest, sea water, soy sauce and isotonic drinks.Fil: Lancioni, Carlina. Universidad Nacional de la Plata. Facultad de Cs.exactas. Laboratorio de Investigacion y Desarrollo de Metodos Analiticos. - Comision de Investigaciones Cientificas de la Provincia de Buenos Aires. Laboratorio de Investigacion y Desarrollo de Metodos Analiticos.; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata; ArgentinaFil: Aspromonte, Juan. Universidad Nacional de la Plata. Facultad de Cs.exactas. Laboratorio de Investigacion y Desarrollo de Metodos Analiticos. - Comision de Investigaciones Cientificas de la Provincia de Buenos Aires. Laboratorio de Investigacion y Desarrollo de Metodos Analiticos.; Argentina. Katholikie Universiteit Leuven; Bélgica. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata; ArgentinaFil: Tascon, Marcos. Universidad Nacional de San Martín. Instituto de Investigación e Ingeniería Ambiental. - Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Instituto de Investigación e Ingeniería Ambiental; ArgentinaFil: Gagliardi, Leonardo Gabriel. Universidad Nacional de la Plata. Facultad de Cs.exactas. Laboratorio de Investigacion y Desarrollo de Metodos Analiticos. - Comision de Investigaciones Cientificas de la Provincia de Buenos Aires. Laboratorio de Investigacion y Desarrollo de Metodos Analiticos.; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - La Plata; Argentin

A high performance system to study the influence of temperature in on-line solid-phase extraction capillary electrophoresis

A novel high performance system to control the temperature of the microcartridge in on-line solid phase extraction capillary electrophoresis (SPE–CE) is introduced. The mini-device consists in a thermostatic bath that fits inside of the cassette of any commercial CE instrument, while its temperature is controlled from an external circuit of liquid connecting three differentwater baths. The circuits are controlled from a switchboard connected to an array of electrovalves that allow to rapidly alternate the water circulation through the mini-thermostatic-bath between temperatures from 5 to 90 ºC. The combination of the mini-device and the forced-air thermostatization system of the commercial CE instrument allows to optimize independently the temperature of the sample loading, the clean-up, the analyte elution and the electrophoretic separation steps. The system is used to study the effect of temperature on the C18-SPE–CE analysis of the opioid peptides, Dynorphin A (Dyn A), Endomorphin1 (END) and Met-enkephalin (MET), in both standard solutions and in spiked plasma samples. Extraction recoveries demonstrated to depend, with a non-monotonous trend, on the microcartridge temperature during the sample loading and became maximum at 60 ºC. Results prove the potential of temperature control to further enhance sensitivity in SPE–CE when analytes are thermally stable.Facultad de Ciencias ExactasLaboratorio de Investigación y Desarrollo de Métodos Analíticos (LIDMA)Centro de Investigación y Desarrollo en Tecnología de Pintura

Measurement of Free Drug Concentration from Biological Tissue by Solid-Phase Microextraction: In Silico and Experimental Study

In this article, the use of an SPME technique is reported for the first time for direct measurement of free drug concentration in solid tissue. In our investigations, we considered doxorubicin (DOX) spiked in homogenized tissue matrix at transient and equilibrium extraction conditions, with subsequent assessment of obtained experimental results by an in silico approach using mathematical models developed in COMSOL Multyphysics. In silico studies were performed on the basis of transported diluted species (tds) and reaction engineering (re) modules from COMSOL Multiphysics, using the same conditions as those used to attain experimental results. To determine the apparent binding affinity of DOX to the tissue matrix which contains multiple binding species, the experimentally determined binding affinity of DOX with human serum albumin (HSA) was considered to simplify the mathematical calculations. Here, the value of the binding affinity was considered for a single binding site and adjusted by fitting the experimental results with the mathematical model. Bovine lung tissue homogenate was selected as a surrogate matrix, and a biocompatible C-8 commercial SPME fiber was used for extraction of DOX. In total, four mathematical models were herein developed to describe the mass transfer kinetics of solid coatings: in agar gel at static conditions, in PBS solution with agitated conditions, extraction in PBS solution in the presence of an HSA binding matrix, and static extraction in homogenized lung tissue. For all conditions, simulated results were in good agreement with experimental results. The developed mathematical model allows for measurements of free drug concentrations inside the tissue matrix and facilitates calculations of local depletion of DOX by a solid SPME coating. Results of the investigations indicate that local depletion of the free form of DOX, even at the kinetic stage, is negligible for tissue extraction, as the release of the heavily bound analyte (over 99% binding to tissue matrix) is very rapid, thus easily compensating for the loss of the drug to the SPME coating. This indicates that the dissociation rate constant of DOX from lung tissue components is very rapid; therefore, the mass transfer of drug to the fiber coating via free from is very efficient. Our results also indicate that thin coating SPME fibers provide a good way to measure drug distribution after dosing, as extractions via thin coating SPME fibers do not affect the free concentration of the drug, which is responsible for drug distribution in tissue.Fil: Huq, Mohammad. University of Waterloo; CanadáFil: Tascon, Marcos. University of Waterloo; Canadá. Universidad Nacional de San Martín. Instituto de Investigación e Ingeniería Ambiental. - Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Instituto de Investigación e Ingeniería Ambiental; ArgentinaFil: Nazdrajic, Emir. University of Waterloo; CanadáFil: Roszkowska, Anna. University of Waterloo; CanadáFil: Pawliszyn, Janusz. University of Waterloo; Canad

Looking for paint mixtures to glimpse pictorial techniques: a micro-stratigraphic physicochemical approach to the rock art from the Oyola’s Caves (Argentina)

Could not be possible that rock paintings with similar hues and morphologies were the result of different paint preparations inside a cave but distanced in time? Is there any archaeometric approach that allow us to evidence these subtle differences? Aiming to address these inquires, in this work are presented the potentials of new physicochemical lines of evidence for characterization and differentiation of paint mixtures. This will improve the understanding of the technical heterogeneity and temporal complexity of painting sets executed in a particular archaeological site. In order to explore these points, the results obtained in the micro-stratigraphic studies of samples taken from the painted walls of Oyola, an archaeological site located in the northwest of Argentina, are presented. These samples have been analyzed by micro-Raman spectroscopy (mRS) and scanning electron microscopy with energy dispersive X-ray (SEM–EDS). The differences found by cross-section chemical studies could be explained as a consequence of two situations: 1-differences in the painting’s chemical components, either in the pigments involved or additives used; and, 2-differences in the physical properties of the mixtures such as stratum thickness and/or particle size. Also, in this article are explained each of the hypothesis, presenting the limits of these interpretations and pointing out future research challenges. As we discussed, it could be possible that the chemical and physical differences found between paint mixtures were the material expression of varied types of pictorial techniques.Fil: Gheco, Lucas Ignacio. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro de Investigaciones y Transferencia de Catamarca. Universidad Nacional de Catamarca. Centro de Investigaciones y Transferencia de Catamarca; Argentina. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; ArgentinaFil: Tascon, Marcos. Universidad Nacional de San Martín. Instituto de Investigación e Ingeniería Ambiental. - Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Instituto de Investigación e Ingeniería Ambiental; ArgentinaFil: Ahets Etcheberry, Eugenia Inés. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; ArgentinaFil: Quesada, Marcos Nicolás. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro de Investigaciones y Transferencia de Catamarca. Universidad Nacional de Catamarca. Centro de Investigaciones y Transferencia de Catamarca; ArgentinaFil: Marte, Fernando. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; Argentin

A rapid and simple method for the determination of psychoactive alkaloids by CE-UV: application to Peganum Harmala seed infusions

The β-carboline alkaloids of the harmala (HAlks) group are compounds widely spread in many natural sources, but found at relatively high levels in some specific plants like Peganum harmala (Syrian rue) or Banisteriopsis caapi. HAlks are a reversible Mono Amino Oxidase type A Inhibitor (MAOI) and, as a consequence, these plants or their extracts can be used to produce psychotropic effects when are combined with psychotropic drugs based on amino groups. Since the occurrence and the levels of the HAlks in natural sources are subject to significant variability, more widespread use is not clinical but recreational or ritual, for example B. caapi is a known part of the Ayahuasca ritual mixture. The lack of simple methods to control the variable levels of these compounds in natural sources restricts the possibilities to dose in strict quantities and, as a consequence, limits its use with pharmacological or clinical purposes. In this work, we present a fast, simple, and robust method of quantifying simultaneously the six HAlksmore frequently found in plants, i.e., harmine, harmaline, harmol, harmalol, harmane, and norharmane, by capillary electrophoresis instruments equipped with the more common detector UV. The method is applied to analyze these HAlks in P. Harmala seeds infusion which is a frequent intake form for these HAlks. The method is validated in three different instruments in order to evaluate the transferability and to compare the performances between them. In this case, harmaline, harmine, and harmol were found in the infusion samples.Laboratorio de Investigación y Desarrollo de Métodos Analíticos (LIDMA

Hidden paintings, forgotten histories: a micro-stratigraphic approach to study coated rock art

Is it possible to detect rock paintings coated by natural or anthropic concretions? In this work, a methodology to discover and characterize underlying paintings is proposed. This approach combines chemical studies by micro-Raman and SEM-EDS of micro-stratigraphic samples taken from the paintings and support rock. As a case of study, it is described the research performed in the archeological site of Oyola in the northwest of Argentina. Strong evidences of red, black, and white hidden paintings have been found. In addition, the method herein presented is thoroughly evaluated pointing out their possibilities and limitations as a tool for the understanding of the historical processes involving production and transformation of the rock art panels. To this end, the methodology was proofed to be a successful exploratory approach for painting detection, expanding its capabilities when complemented with non-invasive characterization techniques.Fil: Gheco, Lucas Ignacio. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro de Investigaciones y Transferencia de Catamarca. Universidad Nacional de Catamarca. Centro de Investigaciones y Transferencia de Catamarca; Argentina. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; ArgentinaFil: Tascon, Marcos. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; Argentina. Universidad Nacional de San Martín. Instituto de Investigación e Ingeniería Ambiental. - Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Instituto de Investigación e Ingeniería Ambiental; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; ArgentinaFil: Gastaldi, Marcos Roman. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Antropología de Córdoba. Universidad Nacional de Córdoba. Facultad de Filosofía y Humanidades. Instituto de Antropología de Córdoba; ArgentinaFil: Ahets Etcheberry, Eugenia Inés. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; Argentina. Universidad de Buenos Aires. Facultad de Filosofía y Letras; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; ArgentinaFil: Pereda, Soledad. Instituto Nacional de Tecnología Industrial; ArgentinaFil: Mastrangelo, Noemi Elisa. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; ArgentinaFil: Quesada, Marcos Nicolás. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro de Investigaciones y Transferencia de Catamarca. Universidad Nacional de Catamarca. Centro de Investigaciones y Transferencia de Catamarca; Argentina. Universidad Nacional de Catamarca. Escuela de Arqueología; ArgentinaFil: Marte, Fernando Daniel. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; Argentin

About the Vulnerability of Photographic Materials: Degradation of Cellulose Acetate and Development of Microanalytical Tools for its Early Diagnostic

Actualmente, los materiales plásticos de acetato de celulosa conforman algunos de los ejemplares más populares y conflictivos dentro de los acervos culturales, siendo empleados como elemento soporte de fotografías o películas cinematográficas y como parte de otros bienes inscriptos en la esfera patrimonial y del arte moderno-contemporáneo. La problemática respecto a este material radica en que se distingue por padecer un deterioro autocatalítico que se caracteriza por la formación de ácido acético como subproducto de la descomposición. Este fenómeno bien conocido en los archivos se denomina ?síndrome del vinagre? y afecta al soporte con signos de contracción, deformación, exudación de plastificantes, e induciendo deterioro incluso sobre materiales colindantes. El objetivo de este trabajo es contribuir al desarrollo de herramientas de diagnóstico no invasivo y micro-invasivo para el monitoreo del grado de deterioro de soportes de acetato de celulosa. Para ello en primera instancia, a partir de diferentes niveles de análisis, se propone caracterizar tanto la materialidad como también los mecanismos y productos de degradación de muestras envejecidas artificialmente. Los resultados experimentales fueron integrados y se propusieron potenciales marcadores que permitirían estimar el estado de conservación de objetos culturales constituidos por acetato de celulosa.Cellulose acetate-based plastics constitute one of the most popular and conflicting materials in cultural heritage. It is not only used as support in photography and cinematography films but also as part of other cultural objects such as modern-contemporary art pieces. One of the main issues of cellulose acetate is the autocatalytic degradation characterized by the formation of acetic acid as a decomposition byproduct. This well-known phenomenon in archives is called “vinegar syndrome” and affects the support generating film contraction, deformation and exudation of plasticizers, inducing dangerous degradation reactions on surrounding materials. In this sense, the goal of this work is to contribute to the development of non-invasive and micro-invasive diagnostic tools for monitoring the stage of degradation of cellulose acetate supports. To this aim, the workflow consisted of different levels of analysis, allowing to perform a thorough material characterization followed by the elucidation of degradation mechanisms based on artificially aged samples. The experimental results from different techniques were integrated and potential markers were proposed enabling the diagnostic of the state of conservation of cultural objects made of cellulose acetate.Fil: Lopez, Rocio. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; ArgentinaFil: Buongarzoni, Laura Antonella. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; ArgentinaFil: Morales, Ana María. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; ArgentinaFil: Tascon, Marcos. Universidad Nacional de San Martín. Instituto de Investigación e Ingeniería Ambiental. - Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Instituto de Investigación e Ingeniería Ambiental; Argentin

About the Vulnerability of Photographic Materials: Degradation of Cellulose Acetate and Development of Microanalytical Tools for its Early Diagnostic

Actualmente, los materiales plásticos de acetato de celulosa conforman algunos de los ejemplares más populares y conflictivos dentro de los acervos culturales, siendo empleados como elemento soporte de fotografías o películas cinematográficas y como parte de otros bienes inscriptos en la esfera patrimonial y del arte moderno-contemporáneo. La problemática respecto a este material radica en que se distingue por padecer un deterioro autocatalítico que se caracteriza por la formación de ácido acético como subproducto de la descomposición. Este fenómeno bien conocido en los archivos se denomina ?síndrome del vinagre? y afecta al soporte con signos de contracción, deformación, exudación de plastificantes, e induciendo deterioro incluso sobre materiales colindantes. El objetivo de este trabajo es contribuir al desarrollo de herramientas de diagnóstico no invasivo y micro-invasivo para el monitoreo del grado de deterioro de soportes de acetato de celulosa. Para ello en primera instancia, a partir de diferentes niveles de análisis, se propone caracterizar tanto la materialidad como también los mecanismos y productos de degradación de muestras envejecidas artificialmente. Los resultados experimentales fueron integrados y se propusieron potenciales marcadores que permitirían estimar el estado de conservación de objetos culturales constituidos por acetato de celulosa.Cellulose acetate-based plastics constitute one of the most popular and conflicting materials in cultural heritage. It is not only used as support in photography and cinematography films but also as part of other cultural objects such as modern-contemporary art pieces. One of the main issues of cellulose acetate is the autocatalytic degradation characterized by the formation of acetic acid as a decomposition byproduct. This well-known phenomenon in archives is called “vinegar syndrome” and affects the support generating film contraction, deformation and exudation of plasticizers, inducing dangerous degradation reactions on surrounding materials. In this sense, the goal of this work is to contribute to the development of non-invasive and micro-invasive diagnostic tools for monitoring the stage of degradation of cellulose acetate supports. To this aim, the workflow consisted of different levels of analysis, allowing to perform a thorough material characterization followed by the elucidation of degradation mechanisms based on artificially aged samples. The experimental results from different techniques were integrated and potential markers were proposed enabling the diagnostic of the state of conservation of cultural objects made of cellulose acetate.Fil: Lopez, Rocio. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; ArgentinaFil: Buongarzoni, Laura Antonella. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; ArgentinaFil: Morales, Ana María. Universidad Nacional de San Martín. Instituto de Investigaciones sobre el Patrimonio Cultural; ArgentinaFil: Tascon, Marcos. Universidad Nacional de San Martín. Instituto de Investigación e Ingeniería Ambiental. - Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Instituto de Investigación e Ingeniería Ambiental; Argentin