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Prof. Pilar Campíns-Falcó
Department of Analytical Chemistry, Chemistry Faculty, University of Valencia. C/ Doctor Moliner, 50. 46100 Burjassot (Valencia) Spain

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0 Analytical Chemistry
0 Chromatography
0 Environmental Science
0 Health
0 Instrumental Analysis

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Chromatography
In tube solid phase-microextraction
Nanomaterials
Analytical Chemistry
Health
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Sensors and Biosensors

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Journal article
Published: 21 June 2021 in Sensors and Actuators B: Chemical
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Celiac disease is an immune-mediated systemic disorder elicited by gluten and related prolamines in genetically susceptible individuals. The current treatment is a strict and lifelong gluten-free diet. However, compliance with the gluten-free diet is not always adequate and many food products contain low concentrations of gluten. The determination of dietary transgressions is a challenge for patients, physicians and dietitians. Alkylresorcinols (AR) have been proposed as sensitive and specific biomarkers of gluten consumption. In this work silica–polymer composites doped with fast blue B reagent (FB) have been used to estimate alkylresorcinols in biological samples. The proposed colorimetric device was synthetized by immobilizing FB into polydimethylsiloxane-tetraethylortosilicate composite. The assay was based on the spontaneous release of FB to the solution containing AR (3,5-dihydroxyhydrocinnamic acid, DHCA) and the azocomplexe formation (520 nm). The response was evaluated with UV-vis spectroscopy and chromatography (in-tube SPME-Capillary LC-DAD) to isolate DHCA signal. The spectroscopic analysis can be used as a screening tool to differentiate positive and negative samples. Meanwhile, the chromatographic assay was necessary to isolate DHCA response in positive samples. LOD was 60 ng mL -1 by adding a SPE step. Precision provided adequate results (RSD < 15%). Preliminary studies in urine samples displayed successful results, showing DHCA can be used as biomarker of gluten intake. The here proposed methodology clearly simplifies the dietary transgression evaluation thanks to the development of a pre-screening tool before the chromatographic analysis.

ACS Style

L. Hakobyan; M.C. Prieto-Blanco; María Roca Llorens; C. Molins-Legua; M. Fuster-Garcia; Y. Moliner-Martinez; P. Campins-Falcó; Carmen Ribes-Koninckx. Fast blue B functionalized silica-polymer composite to evaluate 3,5-dihydroxyhydrocinnamic acid as biomarker of gluten intake. Sensors and Actuators B: Chemical 2021, 345, 130333 .

AMA Style

L. Hakobyan, M.C. Prieto-Blanco, María Roca Llorens, C. Molins-Legua, M. Fuster-Garcia, Y. Moliner-Martinez, P. Campins-Falcó, Carmen Ribes-Koninckx. Fast blue B functionalized silica-polymer composite to evaluate 3,5-dihydroxyhydrocinnamic acid as biomarker of gluten intake. Sensors and Actuators B: Chemical. 2021; 345 ():130333.

Chicago/Turabian Style

L. Hakobyan; M.C. Prieto-Blanco; María Roca Llorens; C. Molins-Legua; M. Fuster-Garcia; Y. Moliner-Martinez; P. Campins-Falcó; Carmen Ribes-Koninckx. 2021. "Fast blue B functionalized silica-polymer composite to evaluate 3,5-dihydroxyhydrocinnamic acid as biomarker of gluten intake." Sensors and Actuators B: Chemical 345, no. : 130333.

Journal article
Published: 17 June 2021 in Pharmaceuticals
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Dietary supplements of botanical origin are increasingly consumed due to their content of plant constituents with potential benefits on health and wellness. Among those constituents, terpenes are gaining attention because of their diverse biological activities (anti-inflammatory, antibacterial, geroprotective, and others). While most of the existing analytical methods have focused on establishing the terpenic fingerprint of some plants, typically by gas chromatography, methods capable of quantifying representative terpenes in herbal preparations and dietary supplements with combined high sensitivity and precision, simplicity, and high throughput are still necessary. In this study, we have explored the utility of capillary liquid chromatography (CapLC) with diode array detection (DAD) for the determination of different terpenes, namely limonene, linalool, farnesene, α-pinene, and myrcene. An innovative method is proposed that can be applied to quantify the targets at concentration levels as low as 0.006 mg per gram of sample with satisfactory precision, and a total analysis time <30 min per sample. The reliability of the proposed method has been tested by analyzing different dietary supplements of botanical origin, namely three green coffee extract-based products, two fat burnings containing Citrus aurantium (bitter orange), and an herbal preparation containing lime and leaves of orange trees.

ACS Style

Henry Ponce-Rodríguez; Jorge Verdú-Andrés; Pilar Campíns-Falcó; Rosa Herráez-Hernández. Capillary Liquid Chromatography for the Determination of Terpenes in Botanical Dietary Supplements. Pharmaceuticals 2021, 14, 580 .

AMA Style

Henry Ponce-Rodríguez, Jorge Verdú-Andrés, Pilar Campíns-Falcó, Rosa Herráez-Hernández. Capillary Liquid Chromatography for the Determination of Terpenes in Botanical Dietary Supplements. Pharmaceuticals. 2021; 14 (6):580.

Chicago/Turabian Style

Henry Ponce-Rodríguez; Jorge Verdú-Andrés; Pilar Campíns-Falcó; Rosa Herráez-Hernández. 2021. "Capillary Liquid Chromatography for the Determination of Terpenes in Botanical Dietary Supplements." Pharmaceuticals 14, no. 6: 580.

Journal article
Published: 15 June 2021 in Journal of Clinical Medicine
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Purpose: To evaluate and compare corneal hysteresis (CH), corneal resistance factor (CRF), and central corneal thickness (CCT), measurements were taken between a healthy population (controls), patients diagnosed with glaucoma (DG), and glaucoma suspect patients due to ocular hypertension (OHT), family history of glaucoma (FHG), or glaucoma-like optic discs (GLD). Additionally, Goldmann-correlated intraocular pressure (IOPg) and corneal-compensated IOP (IOPcc) were compared between the different groups of patients. Methods: In this prospective analytical-observational study, a total of 1065 patients (one eye of each) were recruited to undergo Ocular Response Analyzer (ORA) testing, ultrasound pachymetry, and clinical examination. Corneal biomechanical parameters (CH, CRF), CCT, IOPg, and IOPcc were measured in the control group (n = 574) and the other groups: DG (n = 147), FHG (n = 78), GLD (n = 90), and OHT (n = 176). We performed a variance analysis (ANOVA) for all the dependent variables according to the different diagnostic categories with multiple comparisons to identify the differences between the diagnostic categories, deeming p< 0.05 as statistically significant. Results: The mean CH in the DG group (9.69 mmHg) was significantly lower compared to controls (10.75 mmHg; mean difference 1.05, p< 0.001), FHG (10.70 mmHg; mean difference 1.00, p< 0.05), GLD (10.63 mmHg; mean difference 0.93, p< 0.05) and OHT (10.54 mmHg; mean difference 0.84, p< 0.05). No glaucoma suspects (FHG, GLD, OHT groups) presented significant differences between themselves and the control group (p = 1.00). No statistically significant differences were found in the mean CRF between DG (11.18 mmHg) and the control group (10.75 mmHg; mean difference 0.42, p = 0.40). The FHG and OHT groups showed significantly higher mean CRF values (12.32 and 12.41 mmHg, respectively) than the DG group (11.18 mmHg), with mean differences of 1.13 (p< 0.05) and 1.22 (p< 0.001), respectively. No statistically significant differences were found in CCT in the analysis between DG (562 μ) and the other groups (control = 556 μ, FHG = 576 μ, GLD = 569 μ, OHT = 570 μ). The means of IOPg and IOPcc values were higher in the DG patient and suspect groups than in the control group, with statistically significant differences in all groups (p< 0.001). Conclusion: This study presents corneal biomechanical values (CH, CRF), CCT, IOPg, and IOPcc for diagnosed glaucoma patients, three suspected glaucoma groups, and a healthy population, using the ORA. Mean CH values were markedly lower in the DG group (diagnosed with glaucoma damage) compared to the other groups. No significant difference was found in CCT between the DG and control groups. Unexpectedly, CRF showed higher values in all groups than in the control group, but the difference was only statistically significant in the suspect groups (FHG, GLD, and OHT), not in the DG group.

ACS Style

Mª. del Buey-Sayas; Elena Lanchares-Sancho; Pilar Campins-Falcó; María Pinazo-Durán; Cristina Peris-Martínez. Corneal Biomechanical Parameters and Central Corneal Thickness in Glaucoma Patients, Glaucoma Suspects, and a Healthy Population. Journal of Clinical Medicine 2021, 10, 2637 .

AMA Style

Mª. del Buey-Sayas, Elena Lanchares-Sancho, Pilar Campins-Falcó, María Pinazo-Durán, Cristina Peris-Martínez. Corneal Biomechanical Parameters and Central Corneal Thickness in Glaucoma Patients, Glaucoma Suspects, and a Healthy Population. Journal of Clinical Medicine. 2021; 10 (12):2637.

Chicago/Turabian Style

Mª. del Buey-Sayas; Elena Lanchares-Sancho; Pilar Campins-Falcó; María Pinazo-Durán; Cristina Peris-Martínez. 2021. "Corneal Biomechanical Parameters and Central Corneal Thickness in Glaucoma Patients, Glaucoma Suspects, and a Healthy Population." Journal of Clinical Medicine 10, no. 12: 2637.

Journal article
Published: 08 June 2021 in Biosensors
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The development of in situ analytical devices has gained outstanding scientific interest. A solid sensing membrane composed of 1,2-naphthoquinone-4-sulfonate (NQS) derivatizing reagent embedded into a polymeric polydimethylsiloxane (PDMS) composite was proposed for in situ ammonium (NH4+) and urea (NH2CONH2) analysis in water and urine samples, respectively. Satisfactory strategies were also applied for urease-catalyzed hydrolysis of urea, either in solution or glass-supported urease immobilization. Using diffuse reflectance measurements combined with digital image processing of color intensity (RGB coordinates), qualitative and quantitative analyte detection was assessed after the colorimetric reaction took place inside the sensing membrane. A suitable linear relationship was found between the sensor response and analyte concentration, and the results were validated by a thymol-PDMS-based sensor based on the Berthelot reaction. The suggested sensing device offers advantages such as rapidity, versatility, portability, and employment of non-toxic reagents that facilitate in situ analysis in an energy-efficient manner.

ACS Style

Adrià Martínez-Aviñó; Lusine Hakobyan; Ana Ballester-Caudet; Yolanda Moliner-Martínez; Carmen Molins-Legua; Pilar Campíns-Falcó. NQS-Doped PDMS Solid Sensor: From Water Matrix to Urine Enzymatic Application. Biosensors 2021, 11, 186 .

AMA Style

Adrià Martínez-Aviñó, Lusine Hakobyan, Ana Ballester-Caudet, Yolanda Moliner-Martínez, Carmen Molins-Legua, Pilar Campíns-Falcó. NQS-Doped PDMS Solid Sensor: From Water Matrix to Urine Enzymatic Application. Biosensors. 2021; 11 (6):186.

Chicago/Turabian Style

Adrià Martínez-Aviñó; Lusine Hakobyan; Ana Ballester-Caudet; Yolanda Moliner-Martínez; Carmen Molins-Legua; Pilar Campíns-Falcó. 2021. "NQS-Doped PDMS Solid Sensor: From Water Matrix to Urine Enzymatic Application." Biosensors 11, no. 6: 186.

Journal article
Published: 21 May 2021 in Analytica Chimica Acta
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Colorimetric localized surface plasmon resonance (LSPR) as analytical response is applied for a wide number of chemical sensors and biosensors. However, the dependence of different factors, such as size distribution of nanoparticles (NPs), shape, dielectric environment, inter-particle distance and matrix, among others, can provide non-reliable results by UV–vis spectrometry in complex matrices if NP assessment is not carried out, particularly at low levels of analyte concentrations. Miniaturized liquid chromatography, capillary (CapLC) and nano (NanoLC), coupled on line with in-tube solid phase microextraction (IT-SPME) is proposed for the first time for both, controlling suitability of used noble metal NP dispersions and developing plasmonic assays. Several capped noble NPs and target analytes were tested from variations in the chromatographic profiles obtained by using diode array detection. The IT-SPME step, which influenced the chromatographic fingerprint provided by noble NP dispersions, was studied by asymmetrical flow field flow fractionation (AF4) too. We monitored NP aggregation induced by interaction with several analytes like acids and spermine (SPN). Assessment of NPs was achieved in less than 10 min and it permitted to develop suitable plasmonic tests. Here, it was also demonstrated that these assays can be followed by IT-SPME-miniaturized LC-DAD and more sensitivity and selectivity than those provided by UV–Vis spectrometry were achieved. Analysing urine samples to determine SPN as a cancer biomarker as a proof of concept is presented.

ACS Style

L. Sanjuan-Navarro; S. Cortés-Bautista; Y. Moliner-Martínez; P. Campíns-Falcó. In-tube solid phase microextraction coupled to miniaturized liquid chromatography for both, noble metal nanoparticle assessment and sensitive plasmonic assay development. Analytica Chimica Acta 2021, 1171, 338665 .

AMA Style

L. Sanjuan-Navarro, S. Cortés-Bautista, Y. Moliner-Martínez, P. Campíns-Falcó. In-tube solid phase microextraction coupled to miniaturized liquid chromatography for both, noble metal nanoparticle assessment and sensitive plasmonic assay development. Analytica Chimica Acta. 2021; 1171 ():338665.

Chicago/Turabian Style

L. Sanjuan-Navarro; S. Cortés-Bautista; Y. Moliner-Martínez; P. Campíns-Falcó. 2021. "In-tube solid phase microextraction coupled to miniaturized liquid chromatography for both, noble metal nanoparticle assessment and sensitive plasmonic assay development." Analytica Chimica Acta 1171, no. : 338665.

Journal article
Published: 20 April 2021 in Talanta
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Scopolamine (SCP) is often involved in sexual assaults and robberies, particularly in recreational environments. Therefore, analytical tools are required for the analysis of this compound amenable for the field. In this work, a sensor for SCP is described based on the entrapment of KMnO4 into polydimethylsiloxane (PDMS). The possibility of using KMnO4 in combination with the reagent 1,2-naphtoquinone-4-sulfonate (NQS) giving a double sensor acting as a bicolorimetric device is also demonstrated. In contact with the sample, the PDMS composite delivers MnO4−, which reacts rapidly with SCP under basic conditions causing a change of the color of the solution that can be related to the concentration of drug using both, absorbances and color coordinates, while the NQS part of the sensor remains unchanged. After an exposure time to the sensors of 10 min, satisfactory linearity was obtained for concentrations of SCP up to 865 μg/mL, being the limit of detection (LOD) 108 μg/mL. A method using a portable nano liquid chromatograph with detection at 255 nm has been also developed; in this case the LOD was 100 μg/mL and the working linear interval was 250–2000 μg/mL. The precision, expressed as relative standard deviation (RDS), was ≤8% for both methods. Different beverages (cola, cola-whisky, tonic water-vodka, red wine and green tea) were assayed. The potential of the two proposed approaches for on-site tests is discussed.

ACS Style

N. Jornet-Martínez; R. Herráez-Hernández; P. Campíns-Falcó. Scopolamine analysis in beverages: Bicolorimetric device vs portable nano liquid chromatography. Talanta 2021, 232, 122406 .

AMA Style

N. Jornet-Martínez, R. Herráez-Hernández, P. Campíns-Falcó. Scopolamine analysis in beverages: Bicolorimetric device vs portable nano liquid chromatography. Talanta. 2021; 232 ():122406.

Chicago/Turabian Style

N. Jornet-Martínez; R. Herráez-Hernández; P. Campíns-Falcó. 2021. "Scopolamine analysis in beverages: Bicolorimetric device vs portable nano liquid chromatography." Talanta 232, no. : 122406.

Journal article
Published: 05 April 2021 in Nanomaterials
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Asymmetrical flow field-flow fractionation (AF4) coupled to UV-Vis and dynamic light scattering (DLS) detectors in series, was tested for stability studies of dispersions of citrate-capped silver nanoparticles (AgNPs) in several water matrices. The main goal is to provide knowledge to understand their possible behavior in the environment for short times since mixturing (up to 180 min). Ultrapure (UPW), bottled (BW1, BW2), tap (TW), transitional (TrW) and sea water (SW) matrices were assayed. Observations were compatible with the aggregation of AgNPs, a change in the plasmon band and a size growth with time were done. Fractograms showed different evolution fingerprints in the function of the waters and batches. The aggregation rate order was BW2, SW, TrW, BW1 and TW, being BW2 the lowest and TW the highest. NP aggregation can be induced by increasing the salt concentration of the medium, however transitional and sea waters did not follow the rule. Both matrices presented a lower aggregation rate in comparison with other aqueous matrices with much lower ionic strength (BW1 and TW), which can be explained by the potential presence of dissolved organic matter and/or the high concentration of halides providing their stabilization and passivation, respectively. AF4 provides relevant information with respect to static DLS and UV-Vis Spectroscopy showing that at least two populations of aggregates with different sizes between them, depending on both, the mixture time for a given matrix and type of water matrix for the same time.

ACS Style

Aaron Boughbina-Portolés; Lorenzo Sanjuan-Navarro; Yolanda Moliner-Martínez; Pilar Campíns-Falcó. Study of the Stability of Citrate Capped AgNPs in Several Environmental Water Matrices by Asymmetrical Flow Field Flow Fractionation. Nanomaterials 2021, 11, 926 .

AMA Style

Aaron Boughbina-Portolés, Lorenzo Sanjuan-Navarro, Yolanda Moliner-Martínez, Pilar Campíns-Falcó. Study of the Stability of Citrate Capped AgNPs in Several Environmental Water Matrices by Asymmetrical Flow Field Flow Fractionation. Nanomaterials. 2021; 11 (4):926.

Chicago/Turabian Style

Aaron Boughbina-Portolés; Lorenzo Sanjuan-Navarro; Yolanda Moliner-Martínez; Pilar Campíns-Falcó. 2021. "Study of the Stability of Citrate Capped AgNPs in Several Environmental Water Matrices by Asymmetrical Flow Field Flow Fractionation." Nanomaterials 11, no. 4: 926.

Research article
Published: 05 April 2021 in Analytical Chemistry
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The analytical information given by different types of instruments was scaled in order to establish suitably the figures of merit of a given methodology based on color measurements. Different lab and portable instruments, including smartphones with and without a miniaturized spectrophotometer accessory, have been tested. In order to obtain broad information and using objective criteria, these instruments have been compared from (1) the analytical point of view, considering mainly the detection limit (limits of detection [LODs]), selectivity, accuracy and intra- and interday precision, size, components, and costs; and (2) the environmental point of view, based on their footprint as kilograms of CO2. No significant differences in the precision were obtained with RSD (%) values lower than 10% for all of the instruments, but the achieved values of LOD, selectivity, accuracy, and cost were different. Footprints of CO2 were better for portable instrumentation, especially for smartphones. Three solid chemosensors made of different materials (PDMS, paper, or nylon) have been tested for the determination of ammonia and hydrogen sulfide at different concentration levels (ppb levels). As a result of this study, some rules for selecting the instrument for obtaining the required information have been established. Two apps have been developed for quantitation by smartphones, one for working with RGB values and the other for spectra obtained by the miniaturized spectrophotometer coupled to a smartphone.

ACS Style

Adria Martínez-Aviño; Carmen Molins-Legua; Campíns-Falcó Pilar. Scaling the Analytical Information Given by Several Types of Colorimetric and Spectroscopic Instruments Including Smartphones: Rules for Their Use and Establishing Figures of Merit of Solid Chemosensors. Analytical Chemistry 2021, 93, 6043 -6052.

AMA Style

Adria Martínez-Aviño, Carmen Molins-Legua, Campíns-Falcó Pilar. Scaling the Analytical Information Given by Several Types of Colorimetric and Spectroscopic Instruments Including Smartphones: Rules for Their Use and Establishing Figures of Merit of Solid Chemosensors. Analytical Chemistry. 2021; 93 (15):6043-6052.

Chicago/Turabian Style

Adria Martínez-Aviño; Carmen Molins-Legua; Campíns-Falcó Pilar. 2021. "Scaling the Analytical Information Given by Several Types of Colorimetric and Spectroscopic Instruments Including Smartphones: Rules for Their Use and Establishing Figures of Merit of Solid Chemosensors." Analytical Chemistry 93, no. 15: 6043-6052.

Journal article
Published: 15 October 2020 in Talanta
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A composite membrane containing 1,2-naphthoquinone-4-sulfonic acid sodium salt (NQS) embedded in an ionic liquid (IL)- polydimethylsiloxane (PDMS)- tetraethyl orthosilicate (TEOS)- SiO2 nanoparticles (NPs) polymeric matrix is proposed. The selected IL was 1-methyl-3-octylimidazolium hexafluorophosphate (OMIM PF6). It is demonstrated that ILs chemical additives of PDMS influenced the sol-gel porosity. The sensor analytical performance for ammonia atmospheres has been tested as a function of sampling time (between 0.5 and 312 h), temperature (25ºC and 4ºC) and sampling volume (between 2L and 22 mL) by means of diffuse reflectance measurements and sensor photos, which can be registered and saved as images by a smartphone, which permit RGB measurements too. Flexible calibration was possible, adapting it to the sampling time, temperature and sampling volume needed for its application. Calibration linear slopes (mA vs ppmv) between 1.7 and 467 ppmv-1 were obtained for ammonia in function of the several studied conditions. Those slopes were between 48 and 91 % higher than those achieved with sensors without ILs. The practical application of this sensing device was demonstrated for the analysis of meat packaging environments, being a potential cost-effective candidate for in situ meat freshness analysis. NQS provided selectivity in reference to other family compounds emitted from meat products, such as sulphides. After 10 days at 4ºC ammonia liberated by the assayed meat was 20 ± 4 μg/kg and 18 ± 3 μg/kg, quantified by using diffuse reflectance and %R measurements, respectively. Homogeneity of the ammonia atmosphere was tested by using two sensors placed in two different positions inside the packages.

ACS Style

A. Ballester-Caudet; L. Hakobyan; Y. Moliner-Martinez; C. Molins-Legua; P. Campíns-Falcó. Ionic-liquid doped polymeric composite as passive colorimetric sensor for meat freshness as a use case. Talanta 2020, 223, 121778 .

AMA Style

A. Ballester-Caudet, L. Hakobyan, Y. Moliner-Martinez, C. Molins-Legua, P. Campíns-Falcó. Ionic-liquid doped polymeric composite as passive colorimetric sensor for meat freshness as a use case. Talanta. 2020; 223 ():121778.

Chicago/Turabian Style

A. Ballester-Caudet; L. Hakobyan; Y. Moliner-Martinez; C. Molins-Legua; P. Campíns-Falcó. 2020. "Ionic-liquid doped polymeric composite as passive colorimetric sensor for meat freshness as a use case." Talanta 223, no. : 121778.

Review article
Published: 14 October 2020 in TrAC Trends in Analytical Chemistry
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Critical and global evaluation of analytical methods should be one of the primary goals in analytical chemistry. A holistic approach, however, requires a look at the varied features: commonly discussed validation criteria, often underrated practical and economic aspects, and typically overlooked compliance with the principles of green analytical chemistry. Carrying out such an assessment in a critical and transparent way is extremely difficult without special tools. The purpose of this work is to discuss and compare the three different approaches that seem to be potential candidates: multi-criteria decision analysis methods (MCDA), HEXAGON, and RGB model. The basic principles of each methodology, individual possibilities offered, and the results of the assessment of selected model methods will be presented. Ultimately, the potential compatibility of assessing the same group of methods using different tools will be examined. This contribution can help to select optimal tool and conduct more thorough and insightful assessments.

ACS Style

Paweł Mateusz Nowak; Paweł Kościelniak; Marek Tobiszewski; Ana Ballester-Caudet; Pilar Campíns-Falcó. Overview of the three multicriteria approaches applied to a global assessment of analytical methods. TrAC Trends in Analytical Chemistry 2020, 133, 116065 .

AMA Style

Paweł Mateusz Nowak, Paweł Kościelniak, Marek Tobiszewski, Ana Ballester-Caudet, Pilar Campíns-Falcó. Overview of the three multicriteria approaches applied to a global assessment of analytical methods. TrAC Trends in Analytical Chemistry. 2020; 133 ():116065.

Chicago/Turabian Style

Paweł Mateusz Nowak; Paweł Kościelniak; Marek Tobiszewski; Ana Ballester-Caudet; Pilar Campíns-Falcó. 2020. "Overview of the three multicriteria approaches applied to a global assessment of analytical methods." TrAC Trends in Analytical Chemistry 133, no. : 116065.

Journal article
Published: 10 September 2020 in Nanomaterials
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Among different nanomaterials, gold and silver nanoparticles (AuNPs and AgNPs) have become useful tools for a wide variety of applications in general, and particularly for plasmonic assays. Particle size and stability analysis are key elements for their practical applications since the NPs properties depend on these parameters. Hence, in the present work, asymmetrical flow field flow fractionation (AF4) coupled to UV-Vis and dynamic light scattering (DLS) detectors in series, has been evaluated for stability studies of citrate-capped AuNPs and AgNPs aqueous dispersions. First, experimental parameters, such as mobile phase or cross-flow rate were optimized. Sodium azide to pH 7 for AuNPs and pH 9.2 for AgNPs were selected as the optimum mobile phase. The analytical response of bulk dispersions of AuNPs (20, 40, 60 and 80 nm) and AgNPs (20, 40 and 60 nm) and their dilutions have been studied. Fractograms showed a decrease on the absorbance signal in diluted dispersions as a function of time and particle size for the diluted dispersions that can be explained by dissolution in diluted dispersion since hydrodynamic diameter was constant. The results indicated that the dependence of the signal with time was more intense for AgNPs than for AuNPs, which can be correlated with its lower stability. These findings should be considered when plasmonic assays are realized. Here, assays involving non-oxidant acidic acids as use cases, were tested for several batches of NPs and considerations about their stability and operability stablished.

ACS Style

Lorenzo Sanjuan-Navarro; Aaron Boughbina-Portolés; Yolanda Moliner-Martínez; Pilar Campíns-Falcó. Aqueous Dilution of Noble NPs Bulk Dispersions: Modeling Instability due to Dissolution by AF4 and Stablishing Considerations for Plasmonic Assays. Nanomaterials 2020, 10, 1802 .

AMA Style

Lorenzo Sanjuan-Navarro, Aaron Boughbina-Portolés, Yolanda Moliner-Martínez, Pilar Campíns-Falcó. Aqueous Dilution of Noble NPs Bulk Dispersions: Modeling Instability due to Dissolution by AF4 and Stablishing Considerations for Plasmonic Assays. Nanomaterials. 2020; 10 (9):1802.

Chicago/Turabian Style

Lorenzo Sanjuan-Navarro; Aaron Boughbina-Portolés; Yolanda Moliner-Martínez; Pilar Campíns-Falcó. 2020. "Aqueous Dilution of Noble NPs Bulk Dispersions: Modeling Instability due to Dissolution by AF4 and Stablishing Considerations for Plasmonic Assays." Nanomaterials 10, no. 9: 1802.

Journal article
Published: 24 July 2020 in Science of The Total Environment
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Analytical performance and optimization of figures of merit of a portable nano liquid chromatograph (NanoLC) with UV detection at 255 nm have been established for in place analysis. Methylxanthines: caffeine, theophylline and theobromine were selected as target analytes. A fast lab method based on IT-SPME coupled on line with capillary liquid chromatograph (CapLC) with diode array detection (DAD) was employed for comparative studies. IT-SPME and solid phase extraction were coupled off-line to NanoLC for improving instrumental parameters, mainly detection capacity and selectivity. IT-SPME or SPE/portable NanoLC based methods were superior in terms of chromatographic resolution and organic solvent consumption per sample, around 200 μL vs 10 mL for IT-SPME-CapLC-DAD. Limits of detection (LODs) obtained with the SPE/portable NanoLC were 2–10 ng/mL, which can be suitable for testing the presence of the analytes in several environmental waters in the field. As predictable, the lab method provided better LODs, between 0.1 and 0.5 ng/mL. Good linearity was achieved for both methods and precision was similar for them (≤7%). Both systems were tested for the analysis of real water samples with suitable results.

ACS Style

H.D. Ponce-Rodríguez; J. Verdú-Andrés; R. Herráez-Hernández; P. Campíns-Falcó. Exploring hand-portable nano-liquid chromatography for in place water analysis: Determination of trimethylxanthines as a use case. Science of The Total Environment 2020, 747, 140966 .

AMA Style

H.D. Ponce-Rodríguez, J. Verdú-Andrés, R. Herráez-Hernández, P. Campíns-Falcó. Exploring hand-portable nano-liquid chromatography for in place water analysis: Determination of trimethylxanthines as a use case. Science of The Total Environment. 2020; 747 ():140966.

Chicago/Turabian Style

H.D. Ponce-Rodríguez; J. Verdú-Andrés; R. Herráez-Hernández; P. Campíns-Falcó. 2020. "Exploring hand-portable nano-liquid chromatography for in place water analysis: Determination of trimethylxanthines as a use case." Science of The Total Environment 747, no. : 140966.

Journal article
Published: 20 June 2020 in Journal of Archaeological Science: Reports
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The funeral chambers of the ancient city of Calakmul (Mexico) and the individuals who were buried in them have brought in recent decades new knowledge about the beliefs and funeral customs of the pre-Hispanic Maya. Tombs and bodies were prepared as part of the rituals that should favor the return of ch'ulel to the Underworld, known as Xibalbá by the ancient Maya. The ch'ulel is one of the two anemic entities that inhabit the individual, equivalent to our concept of the soul. Bodies preparation included coloured scented body ointments application, with a deep symbolic connotation and probably also a conservative purpose. The aim of this research was to characterize pigments and binders used by ancient Maya in body ointments remains in human bones samples from Calakmul Maya archaeological site, and the latter, the physical–chemical identification of organic components mixed with these colours for funeral use, can be considered the great challenge of this research due to the limited results that have been gathered on the subject to date. For this purpose, a multi-analytical approach based on the combination of several non-destructive and micro-destructive analytical techniques has been selected. Pigments were studied by transmitted light optical microscopy, FT-IR spectroscopy in ATR mode, diffuse reflectance UV–VIS spectrometry, and EDX microanalysis provided elemental information in order to find characteristic elements useful to identify the unknown pigments. Surface of the samples was observed with Scanning Electron Microscopy (SEM). Gas-Chromatography coupled with Mass Spectrometry (GC–MS) and Pyrolysis-Gas-Chromatography-Mass Spectrometry (Py-GC-MS) were performed in order to collect information about organic fraction used as binding media. The multi analytical approach identified red pigments as Red Earth (or ochre) and Cinnabar, while the results obtained on organic fractions lead us to suggest the presence of lipidic and gum- based compounds.

ACS Style

Carolina Rigon; Francesca Caterina Izzo; Maria Luisa Vázquez De Ágredos Pascual; Pilar Campíns-Falcó; Henk Van Keulen. New results in ancient Maya rituals researches: The study of human painted bones fragments from Calakmul archaeological site (Mexico). Journal of Archaeological Science: Reports 2020, 32, 102418 .

AMA Style

Carolina Rigon, Francesca Caterina Izzo, Maria Luisa Vázquez De Ágredos Pascual, Pilar Campíns-Falcó, Henk Van Keulen. New results in ancient Maya rituals researches: The study of human painted bones fragments from Calakmul archaeological site (Mexico). Journal of Archaeological Science: Reports. 2020; 32 ():102418.

Chicago/Turabian Style

Carolina Rigon; Francesca Caterina Izzo; Maria Luisa Vázquez De Ágredos Pascual; Pilar Campíns-Falcó; Henk Van Keulen. 2020. "New results in ancient Maya rituals researches: The study of human painted bones fragments from Calakmul archaeological site (Mexico)." Journal of Archaeological Science: Reports 32, no. : 102418.

Journal article
Published: 04 June 2020 in Environmental Pollution
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The presence of ammonium ion in rainwater is due to atmospheric processes which involve its scavenging from gas phase and particulate matter. The fractionated samplings of rainwater can provide information about these processes and their potential sources. However, only a low sample volume may be available, which constrained the analysis in general and more particularly in situ mode. For minimizing this limitation, this work proposes a polydimethylsiloxane (PDMS)-salicylate sensor that produces a color change. The embedding of solid reagents into PDMS was optimized. Good analytical characteristics (analysis time of 10 min, sample volume of 500 μL, limit of detection 0.03 μgmL−1) were obtained. Furthermore, other features of the method such as carbon footprint, equipment cost, residues, toxicity and safety have to be taken into account to be assessed according to the Green Analytical Chemistry approach. In this sense, the hexagon tool was employed for comparing the proposed sensor with methods based on the same reaction as well as with general methods for the ammonium analysis in water (using luminol, ion selective electrode, Nessler and modified Roth method). The proposed method based on PDMS-salicylate sensor stands out from all the others by its sustainability, particularly, in terms of low carbon footprint, residues and cost. The method was applied to fractionated samplings in a suburban site (Galicia, Northwestern Spain) and a higher contribution of the rainout process was observed. When long-duration rain events were analyzed, a relationship between the sampling time and ammonium concentration could indicate a loss of ammonium ion over time. The research focuses on developing an innovative PDMS-sensor, for monitoring ammonium determination in rainwater under wide conditions (scavenging process).

ACS Style

María Carmen Prieto-Blanco; Ana Ballester-Caudet; Francisco Javier Souto-Varela; Purificación López-Mahía; Pilar Campíns-Falcó. Rapid evaluation of ammonium in different rain events minimizing needed volume by a cost-effective and sustainable PDMS supported solid sensor. Environmental Pollution 2020, 265, 114911 .

AMA Style

María Carmen Prieto-Blanco, Ana Ballester-Caudet, Francisco Javier Souto-Varela, Purificación López-Mahía, Pilar Campíns-Falcó. Rapid evaluation of ammonium in different rain events minimizing needed volume by a cost-effective and sustainable PDMS supported solid sensor. Environmental Pollution. 2020; 265 ():114911.

Chicago/Turabian Style

María Carmen Prieto-Blanco; Ana Ballester-Caudet; Francisco Javier Souto-Varela; Purificación López-Mahía; Pilar Campíns-Falcó. 2020. "Rapid evaluation of ammonium in different rain events minimizing needed volume by a cost-effective and sustainable PDMS supported solid sensor." Environmental Pollution 265, no. : 114911.

Review
Published: 25 May 2020 in Molecules
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Over the past years, a great effort has been devoted to the development of new sorbents that can be used to pack or to coat extractive capillaries for in-tube solid-phase microextraction (IT-SPME). Many of those efforts have been focused on the preparation of capillaries for miniaturized liquid chromatography (LC) due to the reduced availability of capillary columns with appropriate dimensions for this kind of system. Moreover, many of the extractive capillaries that have been used for IT-SPME so far are segments of open columns from the gas chromatography (GC) field, but the phase nature and dimensions are very limited. In particular, polar compounds barely interact with stationary GC phases. Capillary GC columns may also be unsuitable when highly selective extractions are needed. In this work, we provide an overview of the extractive capillaries that have been specifically developed for capillary LC (capLC) and nano LC (nanoLC) to enhance the overall performance of the IT-SPME, the chromatographic separation, and the detection. Different monolithic polymers, such as silica C18 and C8 polymers, molecularly imprinted polymers (MIPs), polymers functionalized with antibodies, and polymers reinforced with different types of carbon nanotubes, metal, and metal oxide nanoparticles (including magnetic nanoparticles), and restricted access materials (RAMs) will be presented and critically discussed.

ACS Style

Henry Daniel Ponce-Rodríguez; Jorge Verdú-Andrés; Rosa Herráez-Hernández; Pilar Campíns-Falcó. Innovations in Extractive Phases for In-Tube Solid-Phase Microextraction Coupled to Miniaturized Liquid Chromatography: A Critical Review. Molecules 2020, 25, 2460 .

AMA Style

Henry Daniel Ponce-Rodríguez, Jorge Verdú-Andrés, Rosa Herráez-Hernández, Pilar Campíns-Falcó. Innovations in Extractive Phases for In-Tube Solid-Phase Microextraction Coupled to Miniaturized Liquid Chromatography: A Critical Review. Molecules. 2020; 25 (10):2460.

Chicago/Turabian Style

Henry Daniel Ponce-Rodríguez; Jorge Verdú-Andrés; Rosa Herráez-Hernández; Pilar Campíns-Falcó. 2020. "Innovations in Extractive Phases for In-Tube Solid-Phase Microextraction Coupled to Miniaturized Liquid Chromatography: A Critical Review." Molecules 25, no. 10: 2460.

Research paper
Published: 19 May 2020 in Analytical and Bioanalytical Chemistry
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This paper reports the fabrication and utility of a new solid sensor, which allows the quantitation of silver ions acting as catalyst at the low micromolar level. The optical sensor was prepared by incorporating both reagents, pyrogallol red (PGR) and 1,10-phenanthroline (Phen), in a nylon membrane. The effect of parameters in determining silver-catalyzed oxidation of PGR by persulfate in the presence of Phen as an activator was studied and optimized for achieving suitable sensitivity. Semiquantitative analysis can be performed by visual inspection of the color of the sensor by comparing it with standard responses and quantitative analysis can be carried out by its diffuse reflectance (DR) measurement or by a digital image-processing tool (GIMP) using a smartphone. The sensor exhibited a linear relationship toward Ag(I) concentrations ranging from 0.4 to 10 μM or 1–25 μM and limits of detection of 0.1 μM or 0.3 μM for incubation times of 50 and 30 min, respectively. The relative standard deviation achieved for several batches of sensors was around 2%. The analysis of water samples from tap and refrigerating circuits containing solid biocides, which leach silver ions, prove that this portable and sustainable sensor is successfully operational in real situations. Graphical abstract

ACS Style

Sara Bocanegra-Rodríguez; Neus Jornet-Martínez; Carmen Molins-Legua; Pilar Campíns-Falcó. Portable solid sensor supported in nylon for silver ion determination: testing its liberation as biocide. Analytical and Bioanalytical Chemistry 2020, 412, 4393 -4402.

AMA Style

Sara Bocanegra-Rodríguez, Neus Jornet-Martínez, Carmen Molins-Legua, Pilar Campíns-Falcó. Portable solid sensor supported in nylon for silver ion determination: testing its liberation as biocide. Analytical and Bioanalytical Chemistry. 2020; 412 (18):4393-4402.

Chicago/Turabian Style

Sara Bocanegra-Rodríguez; Neus Jornet-Martínez; Carmen Molins-Legua; Pilar Campíns-Falcó. 2020. "Portable solid sensor supported in nylon for silver ion determination: testing its liberation as biocide." Analytical and Bioanalytical Chemistry 412, no. 18: 4393-4402.

Journal article
Published: 03 March 2020 in Science of The Total Environment
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The degradation kinetics and residual levels of the sulfonylurea herbicide tribenuron-methyl (TBM) in different environmental waters were studied using in tube-solid phase microextraction (IT-SPME) coupled on-line to nano-liquid chromatography (nanoLC) and UV diode array detection (DAD). This approach combines the high extraction efficiency of IT-SPME using polymeric coatings reinforced with metal oxide nanoparticles and the high sensitivity attainable by nanoLC, making possible the determination of TBM at low ppb levels (limit of detection, 0.25 ppb) without altering the sample matrix. The present study demonstrated that the preservation of the sample properties is essential to ensure accurate results at these concentration levels due to the high tendency of TBM to hydrolyze, particularly under the acidic conditions involved in most protocols used for sample treatment. The approach used in the present study was applied to evaluate the degradation of this herbicide under different conditions (UV radiation, pH), as well as to study the evolution of its concentration in different environmental waters, namely sea, river, ditch and transition waters. When the samples were exposed to identical conditions, significant differences in the degradation rate of TBM were found depending on the water matrix. The results obtained indicate that this herbicide can persist from several days to weeks depending on the type of water.

ACS Style

P. Serra-Mora; R. Herráez-Hernández; P. Campíns-Falcó. Minimizing the impact of sample preparation on analytical results: In-tube solid-phase microextraction coupled on-line to nano-liquid chromatography for the monitoring of tribenuron methyl in environmental waters. Science of The Total Environment 2020, 721, 137732 .

AMA Style

P. Serra-Mora, R. Herráez-Hernández, P. Campíns-Falcó. Minimizing the impact of sample preparation on analytical results: In-tube solid-phase microextraction coupled on-line to nano-liquid chromatography for the monitoring of tribenuron methyl in environmental waters. Science of The Total Environment. 2020; 721 ():137732.

Chicago/Turabian Style

P. Serra-Mora; R. Herráez-Hernández; P. Campíns-Falcó. 2020. "Minimizing the impact of sample preparation on analytical results: In-tube solid-phase microextraction coupled on-line to nano-liquid chromatography for the monitoring of tribenuron methyl in environmental waters." Science of The Total Environment 721, no. : 137732.

Research article
Published: 27 January 2020 in ACS Omega
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Herein, we reported a chemiluminescent biosensor based on the covalent immobilization of the horseradish peroxidase (HRP) enzyme on a polydimethylsiloxane (PDMS) support to quantify in situ hydrogen peroxide (H2O2). The chemiluminescent reaction based on the use of luminol as an oxidizable substrate, with HRP as the catalyst, has been used in order to quantify H2O2 as the oxidizing agent. The performance of the proposed biosensor has been demonstrated to determine H2O2 liberated by cells in a culture medium and for evaluating the delivery of H2O2 from denture cleaner tablets, as examples of application. For both analyses, the results indicated that the biosensor is cost-effective, sensitive, and selective with a detection limit of 0.02 μM and good linearity over the range 0.06–10 μM. Precision was also satisfactory (relative standard deviation, % RSD < 6). The strength of this biosensing system is the simplicity, portability, and reusability of the devices; it can be applied up to 60 times with 90% of its activity maintained.

ACS Style

Sara Bocanegra-Rodríguez; Neus Jornet-Martínez; Carmen Molins-Legua; Pilar Campíns-Falcó. New Reusable Solid Biosensor with Covalent Immobilization of the Horseradish Peroxidase Enzyme: In Situ Liberation Studies of Hydrogen Peroxide by Portable Chemiluminescent Determination. ACS Omega 2020, 5, 2419 -2427.

AMA Style

Sara Bocanegra-Rodríguez, Neus Jornet-Martínez, Carmen Molins-Legua, Pilar Campíns-Falcó. New Reusable Solid Biosensor with Covalent Immobilization of the Horseradish Peroxidase Enzyme: In Situ Liberation Studies of Hydrogen Peroxide by Portable Chemiluminescent Determination. ACS Omega. 2020; 5 (5):2419-2427.

Chicago/Turabian Style

Sara Bocanegra-Rodríguez; Neus Jornet-Martínez; Carmen Molins-Legua; Pilar Campíns-Falcó. 2020. "New Reusable Solid Biosensor with Covalent Immobilization of the Horseradish Peroxidase Enzyme: In Situ Liberation Studies of Hydrogen Peroxide by Portable Chemiluminescent Determination." ACS Omega 5, no. 5: 2419-2427.

Journal article
Published: 19 December 2019 in Journal of Chromatography A
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Polymers obtained from tetraethyl orthosilicate (TEOS) and triethoxymethylsilane (MTEOS) have been functionalized with different metal and metal oxide nanoparticles (NPs), and used as coatings of extractive capillaries for the extraction of polar compounds by in-tube solid-phase microextraction (IT-SPME) coupled on-line to nano-liquid chromatography (nano-LC). The extraction capabilities of the new phases have been studied using several triazinic herbicides with log of octanol/water partition coefficients (Kow) ranging from -0.7 to 3.21 under reversed phase chromatographic conditions. Best extraction efficiencies for the most polar compounds (log Kow ≤ 2.3) were typically obtained with the CuO NPs doped phase. The TEOS-MTEOS polymer can be modified with two types of NPs in order to obtain extractive phases capable of interacting with compounds of a wide range of polarities; alternatively, two capillaries each with a different type of NPs can be combined in series with the same goal. Under the later approach the limits of detection (LODs) found for the tested herbicides were 0.02-1.5 µg/L, and the precision expressed as relative standard deviation (RSD) varied from 2 to 10 % (n=3). The recoveries found in sea water samples ranged from 80 to 107 %. In addition, the developed CuO NPs doped phase can be used in hydrophilic interaction chromatography (HILIC), which is the separation mode recommended for highly polar compounds. This has been illustrated using the amino acids tyrosine (log Kow = -2.26) and tryptophan (log Kow = -1.06) as model compounds, being their respective LOD 0.1 and 0.3 µg/mL. Examples of application of the developed bimodal extractive phase to different environmental and waste waters are given in order to show its utility and versatility.

ACS Style

P. Serra-Mora; R. Herráez-Hernández; P. Campíns-Falcó. Bimodal copper oxide nanoparticles doped phase for the extraction of highly polar compounds by in-tube solid-phase microextraction coupled on-line to nano-liquid chromatography. Journal of Chromatography A 2019, 1617, 460819 .

AMA Style

P. Serra-Mora, R. Herráez-Hernández, P. Campíns-Falcó. Bimodal copper oxide nanoparticles doped phase for the extraction of highly polar compounds by in-tube solid-phase microextraction coupled on-line to nano-liquid chromatography. Journal of Chromatography A. 2019; 1617 ():460819.

Chicago/Turabian Style

P. Serra-Mora; R. Herráez-Hernández; P. Campíns-Falcó. 2019. "Bimodal copper oxide nanoparticles doped phase for the extraction of highly polar compounds by in-tube solid-phase microextraction coupled on-line to nano-liquid chromatography." Journal of Chromatography A 1617, no. : 460819.

Journal article
Published: 10 November 2019 in Molecules
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A method has been developed for the separation and quantification of terpenic compounds typically used as markers in the chemical characterization of resins based on capillary liquid chromatography coupled to UV detection. The sample treatment, separation and detection conditions have been optimized in order to analyze compounds of different polarities and volatilities in a single chromatographic run. The monoterpene limonene and the triterpenes lupeol, lupenone, β-amyrin, and α-amyrin have been selected as model compounds. The proposed method provides linear responses and precision (expressed as relative standard deviations) of 0.6% to 17%, within the 0.5–10.0 µg mL−1 concentration interval; the limits of detection (LODs) and quantification (LOQs) were 0.1–0.25 µg mL−1 and 0.4–0.8 µg mL−1, respectively. The method has been applied to the quantification of the target compounds in microsamples. The reliability of the proposed conditions has been tested by analyzing three resins, white copal, copal in tears, and ocote tree resin. Percentages of the triterpenes in the range 0.010% to 0.16% were measured using sample amounts of 10–15 mg, whereas the most abundant compound limonene (≥0.93%) could be determined using 1 mg portions of the resins. The proposed method can be considered complementary to existing protocols aimed at establishing the chemical fingerprint of these kinds of samples.

ACS Style

H. D. Ponce-Rodríguez; R. Herráez-Hernández; J. Verdú-Andrés; P. Campíns-Falcó. Quantitative Analysis of Terpenic Compounds in Microsamples of Resins by Capillary Liquid Chromatography. Molecules 2019, 24, 4068 .

AMA Style

H. D. Ponce-Rodríguez, R. Herráez-Hernández, J. Verdú-Andrés, P. Campíns-Falcó. Quantitative Analysis of Terpenic Compounds in Microsamples of Resins by Capillary Liquid Chromatography. Molecules. 2019; 24 (22):4068.

Chicago/Turabian Style

H. D. Ponce-Rodríguez; R. Herráez-Hernández; J. Verdú-Andrés; P. Campíns-Falcó. 2019. "Quantitative Analysis of Terpenic Compounds in Microsamples of Resins by Capillary Liquid Chromatography." Molecules 24, no. 22: 4068.