Determination of dichlobenil and its major metabolite (BAM) in onions by PTV–GC–MS using PARAFAC2 and experimental design methodology

The optimization of a GC–MS analytical procedure which includes derivatization, Quick Easy Cheap Effective Rugged and Safe (QuEChERS) and programmed temperature vaporization (PTV) using design of experiments is performed to determine 2,6-dichlorobenzonitrile (dichlobenil) and 2,6-dichlorobenzamide (BAM) in onions, using 3,5-dichlorobenzonitrile and 2,4-dichlorobenzamide as internal standards. The use of a central composite design and two D-optimal designs, together with the desirability function, makes it possible to significantly reduce the economic, time and environmental cost of the study. The usefulness of PARAFAC2 for solving problems as the interference of unexpected derivatization artifacts unavoidably linked to some derivatization agents, or the presence of coeluents from the complex matrix, which share m/z ratios with the target compounds, is shown. The limits of decision (CCα) of the optimized procedure, 5.00 μg kg− 1 for dichlobenil and 1.55 μg kg− 1 for BAM (α = 0.05), are below the maximum residue limit (MRL) established by the EU for dichlobenil (20 μg kg− 1) in this commodity.Ministerio de Economía y Competitividad (CTQ2011-26022) and Junta de Castilla y León (BU108A11-2

Identification and quantification of carbamate pesticides in dried lime tree flowers by means of excitation-emission molecular fluorescence and parallel factor analysis when quenching effect exists

A non-separative, fast and inexpensive spectrofluorimetric method based on the second order calibration of excitation-emission fluorescence matrices (EEMs) was proposed for the determination of carbaryl, carbendazim and 1-naphthol in dried lime tree flowers. The trilinearity property of three-way data was used to handle the intrinsic fluorescence of lime flowers and the difference in the fluorescence intensity of each analyte. It also made possible to identify unequivocally each analyte. Trilinearity of the data tensor guarantees the uniqueness of the solution obtained through parallel factor analysis (PARAFAC), so the factors of the decomposition match up with the analytes. In addition, an experimental procedure was proposed to identify, with three-way data, the quenching effect produced by the fluorophores of the lime flowers. This procedure also enabled the selection of the adequate dilution of the lime flowers extract to minimize the quenching effect so the three analytes can be quantified. Finally, the analytes were determined using the standard addition method for a calibration whose standards were chosen with a D-optimal design. The three analytes were unequivocally identified by the correlation between the pure spectra and the PARAFAC excitation and emission spectral loadings. The trueness was established by the accuracy line “calculated concentration versus added concentration” in all cases. Better decision limit values (CCα), in x0 = 0 with the probability of false positive fixed at 0.05, were obtained for the calibration performed in pure solvent: 2.97 μg L−1 for 1-naphthol, 3.74 μg L−1 for carbaryl and 23.25 μg L−1 for carbendazim. The CCα values for the second calibration carried out in matrix were 1.61, 4.34 and 51.75 μg L−1 respectively; while the values obtained considering only the pure samples as calibration set were: 2.65, 8.61 and 28.7 μg L−1, respectively.theMinisteriodeEconomíayCompetitividad(CTQ2011-26022) and JuntadeCastillayLeón(BU108A11-2

Standard addition method based on four-way PARAFAC decomposition to solve the matrix interferences in the determination of carbamate pesticides in lettuce using excitation–emission fluorescence data

The simultaneous determination of two carbamate pesticides (carbaryl and carbendazim) and of the degradation product of carbaryl (1-naphthol) in iceberg lettuce was achieved by means of PARAFAC decomposition and excitation–emission fluorescence matrices. A standard addition method for a calibration based on four-way data was applied using different dilutions of the extract from iceberg lettuce as a fourth way that provided the enough variation of the matrix to carry out the four-way analysis. A high fluorescent overlapping existed between the three analytes and the fluorophores of the matrix. The identification of two fluorescent matrix constituents through the four-way model enabled to know the matrix contribution in each dilution of the extract. This contribution was subtracted from the previous signals and a subsequent three-way analysis was carried out with the tensors corresponding to each dilution. The PARAFAC decomposition of these resulting tensors showed a CORCONDIA index equal to 99%. For the identification of the analytes, the correlation between the PARAFAC spectral loadings and the reference spectra has been used. The trueness of the method, in the concentration range studied, was guaranteed because there was neither constant nor proportional bias according to the appropriate hypothesis tests. The best recovery percentages were obtained with the data from the most diluted extract, being the results: 127.6% for carbaryl, 125.55% for carbendazim and 87.6% for 1-naphthol. When the solvent calibration was performed, the decision limit (CCα) and the capability of detection (CCβ) values, in x0=0, were 2.21 and 4.38 μg L−1 for carbaryl, 4.87 and 9.64 μg L−1 for carbendazim; and 3.22 and 6.38 μg L−1 for 1-naphthol, respectively, for probabilities of false positive and false negative fixed at 0.05. However, these values were 5.30 and 10.49 μg L−1 for carbaryl, 18.05 and 35.73 μg L−1 for carbendazim; and 1.92 and 3.79 μg L−1 for 1-naphthol, respectively, when the matrix-matched calibration using the most diluted extract was carried out in the recovery study.Ministerio de Economía y Competitividad(CTQ2011-26022) and JuntadeCastillayLeón(BU108A11-2)

Robustness testing in the determination of seven drugs in animal muscle by liquid chromatography–tandem mass spectrometry

In this work, the robustness of the sample preparation procedure for the determination of six tranquilizers (xylazine, azaperone, propionylpromazine, chlorpromazine, haloperidol, and azaperol) and a beta-blocker (carazolol) in animal muscle by LC/MS–MS was assessed through the experimental design methodology. A 2III7 − 4 fractional factorial design was performed to evaluate the influence of seven variables on the final concentration of the seven drugs in the samples, in accordance with what is laid down in Commission Decision No 2002/657/EC. The variation considered for each of those seven factors is likely to happen when preparing the samples, being the values chosen as level − 1, the nominal operating conditions. The results of the experimentation were evaluated from different statistical strategies, such as hypothesis testing using an external variance previously estimated, Lenth's method, and Bayesian analysis. Both Lenth's and Bayes' approaches enabled to determine the effect of every variable even though no degrees of freedom were left to estimate the residual error. The same conclusion about the robustness of the extraction step was reached from the three methodologies, namely, none of the seven factors examined influenced on the method performance significantly, so the sample preparation procedure was considered to be robust.Ministerio de Ciencia e Innovación (CTQ2011-26022) and MINECO (CTQ2014- 53157-R)

Prediction of Zamorano cheese quality by near-infrared spectroscopy assessing false non-compliance and false compliance at minimum permitted limits stated by designation of origin regulations

Near-infrared transmittance (NIT) spectroscopy was used to predict the percentage in weight of the fat, dry matter, protein and fat/dry matter contents in Zamorano cheeses, protected with a Designation of Origin by the European Union. A total of 42 cheeses submitted to official control were analysed by reference methods. Samples were scanned (850–1050 nm) and predictive equations were developed using Partial Least Squares regression with a cross-validation step. Eight pretreatments independent from the remaining calibration samples were first considered. The most adequate one was that performing the second derivative (using a Savitzky–Golay method with a nine-point window and a second-order polynomial) followed by the standard normal variate transformation. Percentages of the root mean square error in cross-validation, the coefficient of determination and the mean of the absolute value of relative errors found were, respectively, for fat (0.62; 96.16; 1.05), dry matter (0.76; 96.03; 0.83), protein (0.41; 97.82; 0.81) and the fat/dry matter ratio (0.61; 92.51; 0.66). At a 99% confidence level, the trueness of the NIT+PLS methods for fat, dry matter and protein was verified. The official regulation for Zamorano cheese demands minimum permitted limits on the percentages in weight for protein (25%), dry matter (55%) and the ratio of fat to dry matter (45%). The adaptation of both the decision limit and the detection capability to the case of a minimum permitted limit (CDα and CDβ, respectively) when a Partial Least Squares calibration is used has been applied for the first time for a food product protected by a Designation of Origin. The values of CDα with a probability of false non-compliance equal to 0.05 and of CDβ when, in addition, the probability of false compliance was equal to or less than 0.05, both provided by the corresponding NIT+PLS-based method, were, respectively, for protein (24.78%; 24.57%), dry matter (54.14%; 53.28%) and the fat/dry matter ratio (44.39%; 43.78%).authorsthankthefinancialsupportprovidedbyMinisterio de CienciaeInnovacio´n (CTQ2011-26022)andJuntadeCastillay Leo´n (BU108A11-2

Modelling phenolic and technological maturities of grapes by means of the multivariate relation between organoleptic and physicochemical properties

The ripeness of grapes at the harvest time is one of the most important parameters for obtaining high quality red wines. Traditionally the decision of harvesting is to be taken only after analysing sugar concentration, titratable acidity and pH of the grape juice (technological maturity). However, these parameters only provide information about the pulp ripeness and overlook the real degree of skins and seeds maturities (phenolic maturity). Both maturities, technological and phenolic, are not simultaneously reached, on the contrary they tend to separate depending on several factors: grape variety, cultivar, adverse weather conditions, soil, water availability and cultural practices. Besides, this divergence is increasing as a consequence of the climate change (larger quantities of CO2, less rain, and higher temperatures). 247 samples collected in vineyards representative of the qualified designation of origin Rioja from 2007 to 2011 have been analysed. Samples contain the four grape varieties usual in the elaboration of Rioja wines (‘tempranillo’, ‘garnacha’, ‘mazuelo’ and ‘graciano’). The present study is the first systematic investigation on the maturity of grapes that includes the organoleptic evaluation of the degree of grapes maturity (sugars/acidity maturity, aromatic maturity of the pulp, aromatic maturity of the skins and tannins maturity) together with the values of the physicochemical parameters (probable alcohol degree, total acidity, pH, malic acid, K, total index polyphenolics, anthocyans, absorbances at 420, 520 and 620 nm, colour index and tartaric acid) determined over the same samples. A varimax rotation of the latent variables of a PLS model between the physicochemical variables and the mean of four sensory variables allows identifying both maturities. Besides, the position of the samples in the first plane defines the effect that the different factors exert on both phenolic and technological maturitiesMinisterio de Economía y Competitividad (CTQ2011-26022) and Junta de Castilla y León (BU108A11-2

The comparative responsiveness of Hospital Universitario Princesa Index and other composite indices for assessing rheumatoid arthritis activity

Objective To evaluate the responsiveness in terms of correlation of the Hospital Universitario La Princesa Index (HUPI) comparatively to the traditional composite indices used to assess disease activity in rheumatoid arthritis (RA), and to compare the performance of HUPI-based response criteria with that of the EULAR response criteria. Methods Secondary data analysis from the following studies: ACT-RAY (clinical trial), PROAR (early RA cohort) and EMECAR (pre-biologic era long term RA cohort). Responsiveness was evaluated by: 1) comparing change from baseline (Delta) of HUPI with Delta in other scores by calculating correlation coefficients; 2) calculating standardised effect sizes. The accuracy of response by HUPI and by EULAR criteria was analyzed using linear regressions in which the dependent variable was change in global assessment by physician (Delta GDA-Phy). Results Delta HUPI correlation with change in all other indices ranged from 0.387 to 0.791); HUPI's standardized effect size was larger than those from the other indices in each database used. In ACT-RAY, depending on visit, between 65 and 80% of patients were equally classified by HUPI and EULAR response criteria. However, HUPI criteria were slightly more stringent, with higher percentage of patients classified as non-responder, especially at early visits. HUPI response criteria showed a slightly higher accuracy than EULAR response criteria when using Delta GDA-Phy as gold standard. Conclusion HUPI shows good responsiveness in terms of correlation in each studied scenario (clinical trial, early RA cohort, and established RA cohort). Response criteria by HUPI seem more stringent than EULAR''s

SUPLEMENTO DEL XV CONGRESO INTERNACIONAL DE ACTIVIDAD FÍSICA Y DEPORTE. 17,18 y 19 DE OCTUBRE DEL 2018. ENSENADA, BAJA CALIFORNIA, MÉXICO

Compendio, en formato artículo, de los mejores trabajos presentados en el XV CONGRESO INTERNACIONAL DE ACTIVIDAD FÍSICA Y DEPORTE celebrado los días  17,18 y 19 de octubre del 2018 en la Universidad Autónoma de Baja California en la ciudad de Ensenada, Baja California, México:La nutrición en la actividad física y deportiva: alimentos funcionales con nanotecnología, aplicaciones potenciales. González González, K.Y.; Huerta Plaza, B.A.; Amaya Parra, G. (118-130)Perfil antropométrico, físico y hábitos alimentarios en escolares indígenas de Tijuana México. Avendaño Cano, D.L.; Gómez Miranda, L.M.; Aburto Corona, J.A. (131-142)Relación entre el clima de aprendizaje en Educación Física y la percepción de los estudiantes en las competencias del profesorado. Baños, R; Ortiz-Camacho, M.M.; Baena-Extremera, A.; Granero-Gallegos, A.; Machado-Parra, J.P.; Rentería, I.; Acosta, I.; Ramírez, L. (143-153)Valoración de capacidades físicas, composición corporal y consumo de vitaminas en una competencia de Crossfit. Cervantes-Hernández, N.; Hernández Nájera, N.; Carrasco Legleu, C.E.; Candia Lujan, R.; Enríquez Del Castillo, L.A. (154-164)Relación de la actividad física, características antropométricas y VO2máx en jóvenes universitarios: características por género. Enríquez-del Castillo, L.A.; Cervantes-Hernández, N.; Carrasco-Legleu, C.E.; Candia Luján, R. (165-174)Entrenamiento vibratorio de cuerpo completo y sus efectos sobre la composición corporal en jóvenes universitarios. Flores-Chico, B.; Bañuelos-Teres, L.E.; Buendía Lozada, E.R.P. (175-183)Actualización curricular, plan 2016 de la Licenciatura en Cultura Física de la BUAP. Flores-Chico, B.; Flores-Flores, A.; López de La Rosa, LE.; Aguilar-Enríquez, R.I.; Caballero Gómez, JM; Villanueva-Huerta, JA. (184-192)Evaluación psicológica y de la musculatura isquiosural de basquetbolistas universitarias en distintas etapas deportivas. Moranchel-Charros, R.; Martínez-Velázquez, E.S. (193-203)Efecto del ejercicio físico sobre la fuerza, resistencia y riesgo de caída en mujeres adultas. Ortiz Ortiz, M; Espinoza Gutiérrez, R; Gómez Miranda, LM.; Guzmán Gutiérrez, EC.; Calleja Núñez, JJ. (204-212)Desigualdad vs igualdad numérica y su efecto en la técnica de jugadores de fútbol infantil. Vega-Orozco, SI; Gavotto Nogales, OI; Bernal Reyes, F; Horta Gim, MA; Sarabia Sainz, HM. (213-224

Esperanza condicionada para probabilidades finitamente aditivas

Let (O, ?, J) be a finitely additive probabilistic space formed by any set O, an algebra of subsets ? and a finitely additive probability J. In these conditions, if F belongs to V1(O, ?, J) there exists f, element of the completion of L1(O, ?, J), such that F(E) = ?E f dJ for all E of ? and conversely. The integral representation gives sense to the following result, which is the objective of this paper, in terms of the point function: if ß is a subalgebra of ?, for every F of V1(O, ?, J) there exists a unique element of V1(O, ?, J) which we note down by E(F/ß), conditional expectation of F given ß. E(F/ß) is characterized by (E(F/ß), G) = (F, G) for every G of V8(O, ß, J). Aside from this, the mapping E(./ß): V1(O, ?, J) ? V1(O, ß, J) is lineal, positive, contractive, idempotent and E(J/ß) = J. If F is of Vp(O, ?, J), p > 1, E(F/ß) is of Vp(O, ß,