Final Report Summary - SMART-NANO (Sensitive MeAsuRemenT, detection, and identification of engineered NANOparticles in complex matrices)
Executive Summary:
Nanotechnology is having an increasingly large impact in many industrial sectors, with nanomaterials and engineered nanoparticles (ENPs) being used in many fields, from paints, automotive components, cosmetic products to biology and medicine. It is estimated that every week 3-4 new products containing some form of nanomaterial enter the market and that yearly 1.6 trillion Euros of goods based on nanotechnology are manufactured. The ongoing activities in the legislative arena at EU level on the labelling of ENP-containing consumer products clearly call for cost-effective, practically implementable, robust, highly sensitive, and specific methods for the detection and measurement of nanoparticles. All these attributes are required for the widespread use and acceptance of analytical methods as standards in the industry. The detection, quantification and identification of ENPs are complicated by the complexity and sheer variety of matrices in which ENPs are embedded. For a proper assessment of the fate and potential safety risks associated with nanoparticles, ENPs also need to be detected downstream in matrices as different as waste water sludge, biological systems and soils. The biggest challenge that researchers face today is thus to develop a technology platform that can be used in a wide range of samples and application scenarios with just minimal adjustments and optimizations.
The project SMART-NANO tackled this complex problem by developing an innovative, cost-effective technology platform providing a total solution “from sample-to-result” for the detection, identification, and characterization of engineered nanoparticles (ENPs) in a wide range of matrices. The technology platform is based on a modular and scalable approach, which gives the flexibility to adapt towards new applications with minimal optimization. Four key application fields (Consumer Products, Food, Environment and Biota) were targeted through the development of specific ENP-containing model kits. Parallel to the development of the technology platform, a range of miniaturized, ready-to-use, cost-effective cartridges were developed, together with corresponding analytical protocols.
The SMART-NANO technology platform was extensively tested using ENP-containing kits specifically developed for the four application fields. These tests proved the efficacy of the SMART-NANO platform in detecting and characterizing ENPs in complex matrices, demonstrating significant advantages over currently used techniques. Key innovations introduced by SMART-NANO include the use of reverse supercritical fluid extraction for the treatment of ENP-containing samples, as well as miniaturized, disposable cartridges for flow-field-flow fractionation. Overall, the benchmarking of the SMART-NANO platform confirmed that the platform fulfils the requirements of the application fields in terms of all analyzed parameters (accuracy, reliability, size, sensitivity, repeatability, linearity, LOD and LOQ), while reducing cost, ecological impact and time required for the analysis of complex ENP-containing samples. Most importantly, the presence of nanoparticles in complex samples could be unequivocally demonstrated, and accurate size distribution could be obtained in the vast majority of samples, including the highly relevant case of cosmetic creams.
The SMART-NANO consortium was formed by 8 partners (3 academic and 5 SME’s) from 8 different countries. The balance between industrial and academic partners was one of the key strengths of the project, ensuring the alignment between research efforts and industrial requirements. The results of the SMART-NANO project led to several publications in leading scientific journals and conference presentations. The commercial exploitation of the results has already started with the commercialization of key components of the platform, and will continue with the development of a fully integrated system in the following years.
Project Context and Objectives:
Nanotechnology is having an increasingly large impact in many industrial sectors, with nanomaterials and engineered nanoparticles (ENPs) being used in many fields, from paints, automotive components, consumer products (such as cosmetic sunscreens and anti-odorants) to biology and medicine. It is estimated that every week 3-4 new products containing some form of nanomaterial enter the market and that yearly 1.6 trillion Euros of goods based on nanotechnology are manufactured. The extensive discussions and ongoing activities in the legislative arena at EU level on the labelling of ENP-containing consumer products clearly call for cost-effective, practically implementable, robust, highly sensitive, and specific methods for the detection and measurement of nanoparticles. All these attributes are required for the widespread use and acceptance of analytical methods as standards in the industry. The detection, quantification and identification of ENPs are complicated by the sheer variety and complexity of matrices in which ENPs are embedded, ranging from food, to clothing and cosmetic products. For a proper assessment of the fate and potential safety risks associated with nanoparticles, ENPs also need to be detected downstream in matrices as different as waste water sludge, biological systems and soils. The biggest challenge that researchers face today is thus to develop a technology platform that can be used in a wide range of application scenarios (in terms of embedding matrices and wide range of concentrations) with just minimal adjustments and optimizations for new applications.
The project SMART-NANO tackled this complex problem by developing an innovative, cost-effective technology platform that provides a total solution “from sample-to-result” for the detection, identification, and measurement of engineered nanoparticles (ENPs) in a wide range of matrices. The technology platform is based on a modular and scalable approach, which gives the flexibility to adapt towards new applications with minimal optimization. Four key application fields (Consumer products, Food, Environment and Biota) were targeted through the development of specific model kits containing ENPs. Parallel to the development of the technology platform, analytical methods and protocols have been developed and tested on the developed kits, to ensure ready-to-use, cost-effective cartridges, for immediate, widespread use in real-life applications. The SMART-NANO consortium is formed by 8 partners (3 academic and 5 SME’s) from 8 different countries. The balance between industrial and academic partners was one of the key strengths of the project, ensuring the alignment between research efforts and industrial requirements.
The overall objectives of the SMART-NANO project were defined as follows:
Objective 1: To increase the sensitivity, specificity and versatility of nanoparticle detection instruments using newly developed and optimized pre-separation and separation steps based on ecologically-sound supercritical CO2 extraction and flow field-flow fractionation.
Objective 2: To increase the sensitivity and quantification of nanoparticle detection by next generation dynamic light scattering.
Objective 3: To provide robust, highly sensitive, miniaturized, and application-specific separation and detection cartridges.
Objective 4: To provide innovative hyper-sensitive measurement to assess ENP fate and behavior in complex matrices.
Objective 5: To demonstrate the SMART-NANO detection platform for cost-effective measurements of nanoparticles in complex matrices such as biological systems, consumer products and in the environment.
Objective 6: To guarantee the impact of the project on participating SMEs and the targeted SME dominated industrial communities as well as in the quest for nano-safety evaluation and complete risk assessment of ENP based on actual detected concentrations under various exposure scenarios.
Project Results:
In the framework of SMART-NANO, the following progress could be achieved.
1. Completion of the technology development WPs (WP1-4), i.e. finalization of the technology modules needed for the SMART-NANO platform: sample preparation module (WP1), AF4 size separation module (WP2), UV/MALS optical detection module (WP3), and downstream detection by hDLS and ICP-MS (WP4)
2. Completion of the integration phase (WP5), in which all technology modules from the technology development WPs of the previous periods (WP1-4) were connected and integrated into a single platform.
3. Completion of the application specific protocol optimization (WP6), where the integrated platform was tested and validated with the model ENP kits for cosmetics, food, environment and biota that were developed and prepared during the project.
4. Overall successful completion of the SMART-NANO project, including dissemination activities (WP7) and overall managing tasks (WP8).
The project progress is well in line with the overall objectives of the project listed above:
Progress against Objective 1:
• The consortium demonstrated the efficacy of supercritical CO2 as a widely applicable approach for the ecologically-sound sample preparation of various ENP-containing samples, including highly relevant matrices such as sunscreen and milk.
• Subsequent flow field-flow fractionation yielded an unequivocal verification of the presence of ENPs in complex samples and in most cases allowed a precise determination of the size distribution of ENPs in the sample.
Progress against Objective 2:
• Homodyne DLS was shown to provide improved measurement sensitivity compared to conventional DLS, albeit only in specific conditions.
Progress against Objective 3:
• SMART-NANO managed to miniaturize the 30cm long separation cartridge used today down to less than 7cm, reducing the running time from over 60 minutes down to approximately 20 minutes without significant loss of separation performance.
• The project showed enhanced performance of an improved AF4 separation method based on removing a sample-free fraction of carrier solution, yielding up to 5x increased sensitivity over conventional AF4 methods.
Progress against Objective 4:
• The consortium successfully demonstrated the use of ICP-MS for the hypersensitive identification and partial quantification of ENP in two configurations (off-line and on-line). The detection of TiO2 NP at ppb levels was demonstrated in a model sunscreen matrix in both configurations. The particle size distribution of a polydisperse silver nanoparticles mixture was also demonstrated in the on-line configuration at ppb levels. In addition, single particle detection via ICP-MS allowed detecting silver nanoparticles at ppt levels.
• The limit of detection of UV and MALS-hyphenated AF4 was determined for a range of ENPs in different matrices, as a low cost alternative to ICP-MS, and was found to be suitable for the targeted applications.
Progress against Objective 5:
• The SMART-NANO consortium delivered technology development kits (TDK) of mono-dispersed reference Au, Ag, SiO2 and TiO2 ENPs in water-based matrices, as well as several model specific ENP kits based on incorporating the TDK in complex matrices specific to the 4 model systems. The validation of the platform on these models was successfully completed.
Progress against Objective 6:
• The combination of the ease of use with optimized cartridges and protocols for classes of compounds yields a technology platform that has the potential to be accepted as standard by the ENP industrial community, finally enabling a sound and well defined characterization of nanoparticle ensembles in complex matrices. The impact on the participating SMEs is guaranteed by a detailed exploitation plan targeting the commercialization of several key components of the SMART-NANO platform, in a first stage, and of the complete technology platform in a second stage.
Potential Impact:
The final result of SMART-NANO is an innovative, cost-effective technology platform that provides a total solution “from sample-to-result” for the detection, identification, and measurement of nanoparticles in complex matrices in Consumer Products, Food, the Environment and in situ in Biota. This is expected to have a significant impact in various areas:
Scientific and technical impact:
The innovative technology platform for the detection, identification and measurement of nanoparticles in complex matrices generated high scientific and technical impacts and innovations during the project, and will continue to do so. Innovations such as the use of inverse supercritical fluid extraction and miniaturized/disposable AF4 cartridges shall certainly open new routes for the detection and characterization of nanomaterials.
Economic impact:
SMART-NANO relied on an integrated approach combining knowledge and expertise from both academic, industrial scientists and product developers ensuring the most innovative and practical approaches are explored and investigated. This translated into a series of innovations that is now driving the development of new products. The balance of the consortium between Innovation and Industrialization allowed us to fast-track innovation into products by shifting from a technology push to a market pull.
Policy impact:
SMART-NANO facilitated the complex collaboration required to conduct research and development and to collect end-user requirements, for the benefit of ENPs size measurement, detection and identification. Also due to the direct involvement of JRC, SMART-NANO expects the scientific results to be translated into guidelines and recommendations for control of ENPs in complex matrices. Through its capillary dissemination activities and the interaction with the EU Nano Safety Cluster, SMART-NANO actively promoted its outputs for policy consideration, engaged with the policy makers to inform governmental agencies at an EU-wide and national level.
Societal impact:
SMART-NANO yielded through the consortium partners an EU-wide outreach. It was supported by a combination of partners coming from various ENP-related fields and bringing to the consortium instrumental knowledge about currently running national or regional activities in the field. The innovations achieved by SMART-NANO will have a significant impact on the safety of ENP-based products and on the awareness of European population, as they will set the ground for analyses of a broad range of ENPs in consumer products, food, environment and in biota.
Commercial impact:
Through the participation of leading industrial groups and SMEs, SMART-NANO ensured the alignment between research efforts and industrial requirements. This will enable a smooth transfer of results to products and their rapid introduction into the European and International market. Several of the sectors targeted by our technology platform (cosmetics and personal care, food, environmental sector) see a prevalence of SMEs that would greatly benefit from the availability of an easy-to-use, robust, and cost-effective instrument for the detection, identification, measurement of nanoparticles. SMART-NANO strived to yield as the outcome of the project a validated platform for exploitation by the SME instrument partners. The commercialization of specific components has already started, while the development of an integrated system based on the SMART-NANO platform is planned over the next years.
List of Websites:
www.smartnano.org
Nanotechnology is having an increasingly large impact in many industrial sectors, with nanomaterials and engineered nanoparticles (ENPs) being used in many fields, from paints, automotive components, cosmetic products to biology and medicine. It is estimated that every week 3-4 new products containing some form of nanomaterial enter the market and that yearly 1.6 trillion Euros of goods based on nanotechnology are manufactured. The ongoing activities in the legislative arena at EU level on the labelling of ENP-containing consumer products clearly call for cost-effective, practically implementable, robust, highly sensitive, and specific methods for the detection and measurement of nanoparticles. All these attributes are required for the widespread use and acceptance of analytical methods as standards in the industry. The detection, quantification and identification of ENPs are complicated by the complexity and sheer variety of matrices in which ENPs are embedded. For a proper assessment of the fate and potential safety risks associated with nanoparticles, ENPs also need to be detected downstream in matrices as different as waste water sludge, biological systems and soils. The biggest challenge that researchers face today is thus to develop a technology platform that can be used in a wide range of samples and application scenarios with just minimal adjustments and optimizations.
The project SMART-NANO tackled this complex problem by developing an innovative, cost-effective technology platform providing a total solution “from sample-to-result” for the detection, identification, and characterization of engineered nanoparticles (ENPs) in a wide range of matrices. The technology platform is based on a modular and scalable approach, which gives the flexibility to adapt towards new applications with minimal optimization. Four key application fields (Consumer Products, Food, Environment and Biota) were targeted through the development of specific ENP-containing model kits. Parallel to the development of the technology platform, a range of miniaturized, ready-to-use, cost-effective cartridges were developed, together with corresponding analytical protocols.
The SMART-NANO technology platform was extensively tested using ENP-containing kits specifically developed for the four application fields. These tests proved the efficacy of the SMART-NANO platform in detecting and characterizing ENPs in complex matrices, demonstrating significant advantages over currently used techniques. Key innovations introduced by SMART-NANO include the use of reverse supercritical fluid extraction for the treatment of ENP-containing samples, as well as miniaturized, disposable cartridges for flow-field-flow fractionation. Overall, the benchmarking of the SMART-NANO platform confirmed that the platform fulfils the requirements of the application fields in terms of all analyzed parameters (accuracy, reliability, size, sensitivity, repeatability, linearity, LOD and LOQ), while reducing cost, ecological impact and time required for the analysis of complex ENP-containing samples. Most importantly, the presence of nanoparticles in complex samples could be unequivocally demonstrated, and accurate size distribution could be obtained in the vast majority of samples, including the highly relevant case of cosmetic creams.
The SMART-NANO consortium was formed by 8 partners (3 academic and 5 SME’s) from 8 different countries. The balance between industrial and academic partners was one of the key strengths of the project, ensuring the alignment between research efforts and industrial requirements. The results of the SMART-NANO project led to several publications in leading scientific journals and conference presentations. The commercial exploitation of the results has already started with the commercialization of key components of the platform, and will continue with the development of a fully integrated system in the following years.
Project Context and Objectives:
Nanotechnology is having an increasingly large impact in many industrial sectors, with nanomaterials and engineered nanoparticles (ENPs) being used in many fields, from paints, automotive components, consumer products (such as cosmetic sunscreens and anti-odorants) to biology and medicine. It is estimated that every week 3-4 new products containing some form of nanomaterial enter the market and that yearly 1.6 trillion Euros of goods based on nanotechnology are manufactured. The extensive discussions and ongoing activities in the legislative arena at EU level on the labelling of ENP-containing consumer products clearly call for cost-effective, practically implementable, robust, highly sensitive, and specific methods for the detection and measurement of nanoparticles. All these attributes are required for the widespread use and acceptance of analytical methods as standards in the industry. The detection, quantification and identification of ENPs are complicated by the sheer variety and complexity of matrices in which ENPs are embedded, ranging from food, to clothing and cosmetic products. For a proper assessment of the fate and potential safety risks associated with nanoparticles, ENPs also need to be detected downstream in matrices as different as waste water sludge, biological systems and soils. The biggest challenge that researchers face today is thus to develop a technology platform that can be used in a wide range of application scenarios (in terms of embedding matrices and wide range of concentrations) with just minimal adjustments and optimizations for new applications.
The project SMART-NANO tackled this complex problem by developing an innovative, cost-effective technology platform that provides a total solution “from sample-to-result” for the detection, identification, and measurement of engineered nanoparticles (ENPs) in a wide range of matrices. The technology platform is based on a modular and scalable approach, which gives the flexibility to adapt towards new applications with minimal optimization. Four key application fields (Consumer products, Food, Environment and Biota) were targeted through the development of specific model kits containing ENPs. Parallel to the development of the technology platform, analytical methods and protocols have been developed and tested on the developed kits, to ensure ready-to-use, cost-effective cartridges, for immediate, widespread use in real-life applications. The SMART-NANO consortium is formed by 8 partners (3 academic and 5 SME’s) from 8 different countries. The balance between industrial and academic partners was one of the key strengths of the project, ensuring the alignment between research efforts and industrial requirements.
The overall objectives of the SMART-NANO project were defined as follows:
Objective 1: To increase the sensitivity, specificity and versatility of nanoparticle detection instruments using newly developed and optimized pre-separation and separation steps based on ecologically-sound supercritical CO2 extraction and flow field-flow fractionation.
Objective 2: To increase the sensitivity and quantification of nanoparticle detection by next generation dynamic light scattering.
Objective 3: To provide robust, highly sensitive, miniaturized, and application-specific separation and detection cartridges.
Objective 4: To provide innovative hyper-sensitive measurement to assess ENP fate and behavior in complex matrices.
Objective 5: To demonstrate the SMART-NANO detection platform for cost-effective measurements of nanoparticles in complex matrices such as biological systems, consumer products and in the environment.
Objective 6: To guarantee the impact of the project on participating SMEs and the targeted SME dominated industrial communities as well as in the quest for nano-safety evaluation and complete risk assessment of ENP based on actual detected concentrations under various exposure scenarios.
Project Results:
In the framework of SMART-NANO, the following progress could be achieved.
1. Completion of the technology development WPs (WP1-4), i.e. finalization of the technology modules needed for the SMART-NANO platform: sample preparation module (WP1), AF4 size separation module (WP2), UV/MALS optical detection module (WP3), and downstream detection by hDLS and ICP-MS (WP4)
2. Completion of the integration phase (WP5), in which all technology modules from the technology development WPs of the previous periods (WP1-4) were connected and integrated into a single platform.
3. Completion of the application specific protocol optimization (WP6), where the integrated platform was tested and validated with the model ENP kits for cosmetics, food, environment and biota that were developed and prepared during the project.
4. Overall successful completion of the SMART-NANO project, including dissemination activities (WP7) and overall managing tasks (WP8).
The project progress is well in line with the overall objectives of the project listed above:
Progress against Objective 1:
• The consortium demonstrated the efficacy of supercritical CO2 as a widely applicable approach for the ecologically-sound sample preparation of various ENP-containing samples, including highly relevant matrices such as sunscreen and milk.
• Subsequent flow field-flow fractionation yielded an unequivocal verification of the presence of ENPs in complex samples and in most cases allowed a precise determination of the size distribution of ENPs in the sample.
Progress against Objective 2:
• Homodyne DLS was shown to provide improved measurement sensitivity compared to conventional DLS, albeit only in specific conditions.
Progress against Objective 3:
• SMART-NANO managed to miniaturize the 30cm long separation cartridge used today down to less than 7cm, reducing the running time from over 60 minutes down to approximately 20 minutes without significant loss of separation performance.
• The project showed enhanced performance of an improved AF4 separation method based on removing a sample-free fraction of carrier solution, yielding up to 5x increased sensitivity over conventional AF4 methods.
Progress against Objective 4:
• The consortium successfully demonstrated the use of ICP-MS for the hypersensitive identification and partial quantification of ENP in two configurations (off-line and on-line). The detection of TiO2 NP at ppb levels was demonstrated in a model sunscreen matrix in both configurations. The particle size distribution of a polydisperse silver nanoparticles mixture was also demonstrated in the on-line configuration at ppb levels. In addition, single particle detection via ICP-MS allowed detecting silver nanoparticles at ppt levels.
• The limit of detection of UV and MALS-hyphenated AF4 was determined for a range of ENPs in different matrices, as a low cost alternative to ICP-MS, and was found to be suitable for the targeted applications.
Progress against Objective 5:
• The SMART-NANO consortium delivered technology development kits (TDK) of mono-dispersed reference Au, Ag, SiO2 and TiO2 ENPs in water-based matrices, as well as several model specific ENP kits based on incorporating the TDK in complex matrices specific to the 4 model systems. The validation of the platform on these models was successfully completed.
Progress against Objective 6:
• The combination of the ease of use with optimized cartridges and protocols for classes of compounds yields a technology platform that has the potential to be accepted as standard by the ENP industrial community, finally enabling a sound and well defined characterization of nanoparticle ensembles in complex matrices. The impact on the participating SMEs is guaranteed by a detailed exploitation plan targeting the commercialization of several key components of the SMART-NANO platform, in a first stage, and of the complete technology platform in a second stage.
Potential Impact:
The final result of SMART-NANO is an innovative, cost-effective technology platform that provides a total solution “from sample-to-result” for the detection, identification, and measurement of nanoparticles in complex matrices in Consumer Products, Food, the Environment and in situ in Biota. This is expected to have a significant impact in various areas:
Scientific and technical impact:
The innovative technology platform for the detection, identification and measurement of nanoparticles in complex matrices generated high scientific and technical impacts and innovations during the project, and will continue to do so. Innovations such as the use of inverse supercritical fluid extraction and miniaturized/disposable AF4 cartridges shall certainly open new routes for the detection and characterization of nanomaterials.
Economic impact:
SMART-NANO relied on an integrated approach combining knowledge and expertise from both academic, industrial scientists and product developers ensuring the most innovative and practical approaches are explored and investigated. This translated into a series of innovations that is now driving the development of new products. The balance of the consortium between Innovation and Industrialization allowed us to fast-track innovation into products by shifting from a technology push to a market pull.
Policy impact:
SMART-NANO facilitated the complex collaboration required to conduct research and development and to collect end-user requirements, for the benefit of ENPs size measurement, detection and identification. Also due to the direct involvement of JRC, SMART-NANO expects the scientific results to be translated into guidelines and recommendations for control of ENPs in complex matrices. Through its capillary dissemination activities and the interaction with the EU Nano Safety Cluster, SMART-NANO actively promoted its outputs for policy consideration, engaged with the policy makers to inform governmental agencies at an EU-wide and national level.
Societal impact:
SMART-NANO yielded through the consortium partners an EU-wide outreach. It was supported by a combination of partners coming from various ENP-related fields and bringing to the consortium instrumental knowledge about currently running national or regional activities in the field. The innovations achieved by SMART-NANO will have a significant impact on the safety of ENP-based products and on the awareness of European population, as they will set the ground for analyses of a broad range of ENPs in consumer products, food, environment and in biota.
Commercial impact:
Through the participation of leading industrial groups and SMEs, SMART-NANO ensured the alignment between research efforts and industrial requirements. This will enable a smooth transfer of results to products and their rapid introduction into the European and International market. Several of the sectors targeted by our technology platform (cosmetics and personal care, food, environmental sector) see a prevalence of SMEs that would greatly benefit from the availability of an easy-to-use, robust, and cost-effective instrument for the detection, identification, measurement of nanoparticles. SMART-NANO strived to yield as the outcome of the project a validated platform for exploitation by the SME instrument partners. The commercialization of specific components has already started, while the development of an integrated system based on the SMART-NANO platform is planned over the next years.
List of Websites:
www.smartnano.org