Determinación de fungicidas en vino mediante extracción en fase sólida y crom...Jorge Casado Agrelo
In this work, a reliable and selective procedure for the determination of thirteen fungicides in red and
white wine samples is proposed. Solid-phase extraction (SPE) and liquid chromatography (LC) tandem
mass spectrometry (MS/MS), based on a hybrid quadrupole time-of-flight (QTOF) system, were used
as sample preparation and determination techniques, respectively. Extraction and purification of target
analytes was carried out simultaneously by using a reversed-phase Oasis HLB (200 mg) SPE cartridge
combined with acetonitrile as elution solvent. Fungicides were determined operating the electrospray
source in the positive ionization mode, with MS/MS conditions adjusted to obtain at least two intense
product ions per compound, or registering two transitions per species when a single product was noticed.
High selective MS/MS chromatograms were extracted using a mass window of 20ppms for each product
ion. Considering external calibration as quantification technique, the overall recoveries (accuracy) of the
procedure ranged between 81% and 114% for red and white wine samples (10–20 mL), spiked at different
concentrations between 5 and 100 ngmL−1. Relative standard deviations of the above data stayed below
12% and the limits of quantification (LOQs) of the method, calculated for 10mL of wine, varied between
0.1 ngmL−1 for cyprodinil (CYP) and 0.7 ngmL−1 for myclobutanil (MYC). The optimized method was
applied to seventeen commercial wines produced in Spain and obtained from local supermarkets. Nine
fungicides were determined, at levels above the LOQs of the method, in the above samples. The maximum
concentrations and the highest occurrence frequencies corresponded to metalaxyl (MET) and iprovalicarb
(IPR).
Determinación de fungicidas en vino mediante extracción en fase sólida y crom...Jorge Casado Agrelo
In this work, a reliable and selective procedure for the determination of thirteen fungicides in red and
white wine samples is proposed. Solid-phase extraction (SPE) and liquid chromatography (LC) tandem
mass spectrometry (MS/MS), based on a hybrid quadrupole time-of-flight (QTOF) system, were used
as sample preparation and determination techniques, respectively. Extraction and purification of target
analytes was carried out simultaneously by using a reversed-phase Oasis HLB (200 mg) SPE cartridge
combined with acetonitrile as elution solvent. Fungicides were determined operating the electrospray
source in the positive ionization mode, with MS/MS conditions adjusted to obtain at least two intense
product ions per compound, or registering two transitions per species when a single product was noticed.
High selective MS/MS chromatograms were extracted using a mass window of 20ppms for each product
ion. Considering external calibration as quantification technique, the overall recoveries (accuracy) of the
procedure ranged between 81% and 114% for red and white wine samples (10–20 mL), spiked at different
concentrations between 5 and 100 ngmL−1. Relative standard deviations of the above data stayed below
12% and the limits of quantification (LOQs) of the method, calculated for 10mL of wine, varied between
0.1 ngmL−1 for cyprodinil (CYP) and 0.7 ngmL−1 for myclobutanil (MYC). The optimized method was
applied to seventeen commercial wines produced in Spain and obtained from local supermarkets. Nine
fungicides were determined, at levels above the LOQs of the method, in the above samples. The maximum
concentrations and the highest occurrence frequencies corresponded to metalaxyl (MET) and iprovalicarb
(IPR).
Optimización y aplicación de un procedimiento de dispersión de matriz en fase...Jorge Casado Agrelo
A simplified sample preparation method, based on the matrix solid-phase dispersion technique,
is proposed for the sensitive determination of 15 organic fungicides in vineyard
soils by gas chromatography–mass spectrometry (GC–MS). Under final working conditions,
sieved samples (0.5 g) were blended and dispersed with 2 g of C18 and transferred to a
polypropylene syringe containing 1 g of diatomaceous earth.Analyteswere recovered using
10 mL of ethyl acetate, this extract was concentrated to 1 mL and fungicides determined by
GC–MS, without additional cleanup. The method provided recoveries in the range from 74
to 122% for soils with total carbon contents up to 5.5% and it allowed the use of external
standard as quantification technique. Inter-day precision, given as relative standard deviations,
stayed between 3 and 13%, and the limits of quantification were comprised between
0.6 and 15 ng g−1. Several fungicides were found in the top layer of vineyard soils with the
highest detection frequency and maximum concentration corresponding to iprovalicarb.
Some real samples were also submitted to pressurized liquid extraction. Measured concentrations
were in excellent agreement with those obtained by matrix solid-phase dispersion,
which reinforces the accuracy of the latter methodology.
Determinación de benzotriazoles en muestras de agua mediante microextracción ...Jorge Casado Agrelo
In this work, we investigate the suitability of a commercial available and low cost polyethersufone (PES) sorbent for the microextraction of 1H-benzotriazole (BTri), and four polar derivatives (4 and 5-methyl-1H-benzotriazole, 4-TTri and 5-TTri; 5,6-dimethyl-1H benzotriazole, XTri; and 5-chloro-1H-benzotriazole, 5-ClBTri) from surface and wastewater samples. The performance of liquid chromatography (LC) combined with quadrupole time-of-flight mass spectrometry (QTOF-MS) for the selective determination of target compounds is also discussed. Parameters affecting the efficiency of the microextraction step, such as sample’s pH, ionic strength, stirring speed and extraction lapse of time, and the PES membrane desorption process have been thoroughly investigated. Analytes were extracted from 15 mL samples, containing a 30% of sodium chloride and adjusted at pH 4.5, using a tubular PES sorbent (5 cm length x 0.7 mm o.d., sorbent volume 42 μL). After methanol desorption and solvent exchange, benzotriazoles were determined by LC-MS, with chromatograms extracted using a mass window of 20 ppm, centered in their [M+H]+ ions. The identity of chromatographic peaks was confirmed with accurate ion product scan (MS/MS) spectra. The method provided limits of quantification (LOQs) between 0.005 and 0.1 ng mL-1, and relative recoveries from 81% to 124% (except for XTri in sewage samples, ca. 60%) with associated standard deviations between 2% and 9%. The efficiency of the PES sorbent for the extraction of these compounds has been compared with that attained by stir-bar sorptive extraction (SBSE), with polydimethylsiloxane (PDMS) covered stir bars. The PES polymer achieved significant higher responses (5- to 20-fold) for these polar pollutants. To the best of our knowledge, this research constitutes the first application of both techniques (microextraction using a PES sorbent and LC-QTOF-MS) for benzotriazoles determination in water samples. The method was used to provide data regarding the levels of target compounds in river and urban wastewater samples, including the individual quantification of 4-methyl and 5-methyl-benzotriazole isomers. Obtained results confirmed the ubiquity of benzotriazole, 4-methyl and 5-methyl-benzotriazole in urban wastewater and their incomplete removal at sewage treatment plants
Presentación enfocada a la petrografía orgánica: macerales, clasificación, metodología de análisis y algunas aplicaciones en el industria petrolera. Espero y les sea de interés.
Optimización y aplicación de un procedimiento de dispersión de matriz en fase...Jorge Casado Agrelo
A simplified sample preparation method, based on the matrix solid-phase dispersion technique,
is proposed for the sensitive determination of 15 organic fungicides in vineyard
soils by gas chromatography–mass spectrometry (GC–MS). Under final working conditions,
sieved samples (0.5 g) were blended and dispersed with 2 g of C18 and transferred to a
polypropylene syringe containing 1 g of diatomaceous earth.Analyteswere recovered using
10 mL of ethyl acetate, this extract was concentrated to 1 mL and fungicides determined by
GC–MS, without additional cleanup. The method provided recoveries in the range from 74
to 122% for soils with total carbon contents up to 5.5% and it allowed the use of external
standard as quantification technique. Inter-day precision, given as relative standard deviations,
stayed between 3 and 13%, and the limits of quantification were comprised between
0.6 and 15 ng g−1. Several fungicides were found in the top layer of vineyard soils with the
highest detection frequency and maximum concentration corresponding to iprovalicarb.
Some real samples were also submitted to pressurized liquid extraction. Measured concentrations
were in excellent agreement with those obtained by matrix solid-phase dispersion,
which reinforces the accuracy of the latter methodology.
Determinación de benzotriazoles en muestras de agua mediante microextracción ...Jorge Casado Agrelo
In this work, we investigate the suitability of a commercial available and low cost polyethersufone (PES) sorbent for the microextraction of 1H-benzotriazole (BTri), and four polar derivatives (4 and 5-methyl-1H-benzotriazole, 4-TTri and 5-TTri; 5,6-dimethyl-1H benzotriazole, XTri; and 5-chloro-1H-benzotriazole, 5-ClBTri) from surface and wastewater samples. The performance of liquid chromatography (LC) combined with quadrupole time-of-flight mass spectrometry (QTOF-MS) for the selective determination of target compounds is also discussed. Parameters affecting the efficiency of the microextraction step, such as sample’s pH, ionic strength, stirring speed and extraction lapse of time, and the PES membrane desorption process have been thoroughly investigated. Analytes were extracted from 15 mL samples, containing a 30% of sodium chloride and adjusted at pH 4.5, using a tubular PES sorbent (5 cm length x 0.7 mm o.d., sorbent volume 42 μL). After methanol desorption and solvent exchange, benzotriazoles were determined by LC-MS, with chromatograms extracted using a mass window of 20 ppm, centered in their [M+H]+ ions. The identity of chromatographic peaks was confirmed with accurate ion product scan (MS/MS) spectra. The method provided limits of quantification (LOQs) between 0.005 and 0.1 ng mL-1, and relative recoveries from 81% to 124% (except for XTri in sewage samples, ca. 60%) with associated standard deviations between 2% and 9%. The efficiency of the PES sorbent for the extraction of these compounds has been compared with that attained by stir-bar sorptive extraction (SBSE), with polydimethylsiloxane (PDMS) covered stir bars. The PES polymer achieved significant higher responses (5- to 20-fold) for these polar pollutants. To the best of our knowledge, this research constitutes the first application of both techniques (microextraction using a PES sorbent and LC-QTOF-MS) for benzotriazoles determination in water samples. The method was used to provide data regarding the levels of target compounds in river and urban wastewater samples, including the individual quantification of 4-methyl and 5-methyl-benzotriazole isomers. Obtained results confirmed the ubiquity of benzotriazole, 4-methyl and 5-methyl-benzotriazole in urban wastewater and their incomplete removal at sewage treatment plants
Presentación enfocada a la petrografía orgánica: macerales, clasificación, metodología de análisis y algunas aplicaciones en el industria petrolera. Espero y les sea de interés.
Similar a Item 3: Presentación de los nuevos integrantes de LATSOLAN a través de sus laboratorios Nacionales de Referencia: Nicaragua (20)
Item 9: Soil mapping to support sustainable agricultureExternalEvents
SOIL ATLAS OF ASIA
2ND EDITORIAL BOARD MEETING
RURAL DEVELOPMENT ADMINISTRATION, NATIONAL INSTITUTE OF AGRICULTURAL SCIENCES,
JEONJU, REPUBLIC OF KOREA | 29 APRIL – 3 MAY 2019
Markus Anda (Indonesia)
Item 8: WRB, World Reference Base for Soil ResoucesExternalEvents
SOIL ATLAS OF ASIA
2ND EDITORIAL BOARD MEETING
RURAL DEVELOPMENT ADMINISTRATION, NATIONAL INSTITUTE OF AGRICULTURAL SCIENCES,
JEONJU, REPUBLIC OF KOREA | 29 APRIL – 3 MAY 2019
Satira Udomsri (Thailand)
SOIL ATLAS OF ASIA
2ND EDITORIAL BOARD MEETING
RURAL DEVELOPMENT ADMINISTRATION, NATIONAL INSTITUTE OF AGRICULTURAL SCIENCES,
JEONJU, REPUBLIC OF KOREA | 29 APRIL – 3 MAY 2019
Shree Prasad Vista (Nepal)
Item 6: International Center for Biosaline AgricultureExternalEvents
SOIL ATLAS OF ASIA
2ND EDITORIAL BOARD MEETING
RURAL DEVELOPMENT ADMINISTRATION, NATIONAL INSTITUTE OF AGRICULTURAL SCIENCES,
JEONJU, REPUBLIC OF KOREA | 29 APRIL – 3 MAY 2019
ACERTIJO DE CARRERA OLÍMPICA DE SUMA DE LABERINTOS. Por JAVIER SOLIS NOYOLAJAVIER SOLIS NOYOLA
El Mtro. JAVIER SOLIS NOYOLA, crea y desarrolla ACERTIJO: «CARRERA OLÍMPICA DE SUMA DE LABERINTOS». Esta actividad de aprendizaje lúdico que implica de cálculo aritmético y motricidad fina, promueve los pensamientos lógico y creativo; ya que contempla procesos mentales de: PERCEPCIÓN, ATENCIÓN, MEMORIA, IMAGINACIÓN, PERSPICACIA, LÓGICA LINGUISTICA, VISO-ESPACIAL, INFERENCIA, ETCÉTERA. Didácticamente, es una actividad de aprendizaje transversal que integra áreas de: Matemáticas, Neurociencias, Arte, Lenguaje y comunicación, etcétera.
Today is Pentecost. Who is it that is here in front of you? (Wang Omma.) Jesus Christ and the substantial Holy Spirit, the only Begotten Daughter, Wang Omma, are both here. I am here because of Jesus's hope. Having no recourse but to go to the cross, he promised to return. Christianity began with the apostles, with their resurrection through the Holy Spirit at Pentecost.
Hoy es Pentecostés. ¿Quién es el que está aquí frente a vosotros? (Wang Omma.) Jesucristo y el Espíritu Santo sustancial, la única Hija Unigénita, Wang Omma, están ambos aquí. Estoy aquí por la esperanza de Jesús. No teniendo más remedio que ir a la cruz, prometió regresar. El cristianismo comenzó con los apóstoles, con su resurrección por medio del Espíritu Santo en Pentecostés.
ROMPECABEZAS DE ECUACIONES DE PRIMER GRADO OLIMPIADA DE PARÍS 2024. Por JAVIE...JAVIER SOLIS NOYOLA
El Mtro. JAVIER SOLIS NOYOLA crea y desarrolla el “ROMPECABEZAS DE ECUACIONES DE 1ER. GRADO OLIMPIADA DE PARÍS 2024”. Esta actividad de aprendizaje propone retos de cálculo algebraico mediante ecuaciones de 1er. grado, y viso-espacialidad, lo cual dará la oportunidad de formar un rompecabezas. La intención didáctica de esta actividad de aprendizaje es, promover los pensamientos lógicos (convergente) y creativo (divergente o lateral), mediante modelos mentales de: atención, memoria, imaginación, percepción (Geométrica y conceptual), perspicacia, inferencia, viso-espacialidad. Esta actividad de aprendizaje es de enfoques lúdico y transversal, ya que integra diversas áreas del conocimiento, entre ellas: matemático, artístico, lenguaje, historia, y las neurociencias.
Item 3: Presentación de los nuevos integrantes de LATSOLAN a través de sus laboratorios Nacionales de Referencia: Nicaragua
1. Laboratorio de Suelos y Agua
Comandante Fidel Castro Ruz – LASAF
Instituto Nicaraguense de Tecnología Agropecuaria
INTA
Centro de Desarollo Tecnológico Municipio de
Posoltega, Nicaragua, Región II
2. 1. Personal del laboratorio
Número de empleados: Cinco personas
(tres mujeres, dos
hombres)
Experiencia en análisis de
laboratorio: > 5 años
< 5 años
1 personas
4 personas
Experiencia en gestión de
laboratorios: > 5 años
< 5 años
1 persona
4 personas
3. Ing. Agrónomo : Ronald Torres. Responsable de Laboratorio
Lic. Química: Marnel Membreño, Analista de laboratorio
Ing. Ambientalista: Pedro Muñoz, Analista de laboratorio,
Lic. Química: Estephania López, Analista de laboratorio.
Lic. Química : Alicia Espinoza, Analista de laboratorio
Personal del laboratorio
4. 3. Laboratorios
Oficina de Responsible del Laboratorio
2 ficinas para analistas de Laboratorio
Oficina de Recepción de muestras
Cuarto de pesaje
Cuarto para Análisis de Suelos
Cuarto para Analisis de agua
Cuarto Vestidor para hombres
Cuarto Vestidor para mujeres
Cuarto de Destilador
Cuarto de Reactivos
Cuarto de Cristalería
Cuarto de Secado de Cristaleria
Cuarto de Absorción Atómica
Cuarto de almacenamiento de muestras
Cuarto de reposición de muestras
¿Cuántos m2 de espacio tiene su laboratorio?
(aproximadamente) 620 m2
11. 11
RESULTADOS DE MUESTRAS DE SUELO, 13 muestras - Municipio de Estelí ESTELI – Nicaragua
No.
Cod
Laborat
Descripción
Disponibles MICROS Textura
pH MO N P-disp K Ca Mg CIC Fe Cu Mn Zn
Arcilla Limo Arena
H20 % ppm
meq/100 g suelo
cmol(+)/Kg ppm
1 01-019
Harina de Roca, José Francisco Morales
Morales, Rio Abajo, Pueblo Nuevo, Estelí,
primera 2018 6.9 2.67 0.13 14.09 0.25 14.4 0.63 37.13 0.296N/D 10 2.56 33.28 40 26.72
2 02-019 Fertilizante, José Francisco Morales Morales,
Rio Abajo, Pueblo Nuevo, Estelí, primera 2018 6.9 3.07 0.15 14.57 0.26 21.3 0.89 34.65 N/D N/D 11 0.84 34 38.92 27.08
3 03-019 Testigo, José Francisco Morales Morales, Rio
Abajo, Pueblo Nuevo, Estelí, Primera 2018 6.9 3.18 0.16 8.05 0.26 17.9 0.82 33.66 N/D N/D 8.8 1.44 42.72 36.2 21.08
4 04-019
Harina de Roca, José Francisco Morales
Morales, Rio Abajo, Pueblo Nuevo, Estelí,
postrera 2018 6.8 2.9 0.15 19.55 0.14 27.3 0.77 36.63 N/D N/D 7.7 3.00 36.72 38.2 25.08
5 05-019 Fertilizante, José Francisco Morales Morales,
Rio Abajo, Pueblo Nuevo, Estelí, Postrera 2018 6.8 3.03 0.15 11.31 0.18 20.2 0.63 33.66 0.04N/D 6.1 4.12 40.72 36.2 23.08
6 06-019 Testigo, José Francisco Morales Morales, Rio
Abajo, Pueblo Nuevo, Estelí, Postrera 2018 6.8 3.64 0.18 16.29 0.31 19.8 0.65 34.65 0.78N/D 6.1 0.64 40.72 36.2 23.08
7 07-019 Harina de Roca, José Santos Tercero Los
Copales, Somoto, Madriz, Primera 2018 6.7 3.78 0.19 24.80 0.32 11.2 0.45 17.08 0.576N/D 12 1.00 24.72 38.2 37.08
8 08-019 Fertilizantes, José Santos Tercero Los Copales,
Somoto, Madriz, Primera 2018 6.7 3.44 0.17 29.10 0.21 10.6 0.26 26.24 0.38N/D 9.8 1.55 24.72 38.2 37.08
9 09-019 Testigo, José Santos Tercero Los Copales,
Somoto, Madriz; Primera 2018 6.9 3.52 0.18 26.20 0.36 13.6 0.4 28.71 0.788N/D 8.5 1.92 26.72 34.56 38.72
10 10-019 Harina de Roca, José Santos Tercero Los
Copales, Somoto, Madriz, Postrera 2018 6.7 4.11 0.21 28.90 0.35 17.4 0.41 28.22 0.252N/D 12 3.28 26.72 36.56 36.72
11 11-019 Fertilizantes, José Santos Tercero Los Copales,
Somoto, Madriz, Postrera 2018 6.6 3.89 0.19 50.17 0.52 15.9 0.6 28.71 0.632N/D 14 5.24 22.72 37.28 40
12 12-019 Testigo, José Santos Tercero Los Copales,
Somoto, Madriz, Postrera 2018 6.9 4.08 0.20 57.09 0.23 8.07 0.48 28.71 0.468N/D 22 4.88 22.72 28.72 48.56
13 13-019 Entrada a Estelí, Exdys salinas, La Quinta.
Postrera 2018 6.5 3.33 0.17 65.74 0.14 18.4 0.65 28.22 0.516N/D 9.8 4.48 35.72 31.72 32.56
12. Análisis Físico Químico en Agua
PH
ms/cm
cmol (+)/L
mg/l
mg/l
mg/l
mg/l
mg/l
mg/l
Potenciometrico
Conductivímetro
Absorción atómica
Absorción atómica
Nitrato de plata 0.01 N
,Volumetría
Acido sulfúrico 0.02 N
Volumetría
Cloruro de bario
10%,turbidimetria
Espectrofotometría UV
Absorción atómica; EDTA
Gravimétrico
Parámetro Unidad Método
• PH hidrolítico
• Conductividad Eléctrica
• CI (Calcio, Magnesio, Potasio
y Sodio)
• Elementos menores (Fe, Mn,
Cu, Zn )
• Cloruro
• Alcalinidad(carbonato y
bicarbonato)
• Sulfato
• Nitrato
• Dureza total
• Sólidos totales,sólidos totales
volátiles,sales disueltas
totals,sólidos suspendidos
totals,sólidos disueltos
volátiles y sólidos
suspendidos volátiles.
13. 10. Análisis de suelos en su país
¿Cuántos laboratorios de rutina existen en tu país?
1. LAQUISA - Privado
2. LABSA – Universidad Nacional Agraria - UNA
3. UCATSE – Estelí
4. UNAN -Managua
5. UCA – Universidad Centroamericana
6. UNIAV- Rivas
7. LASAF - INTA
¿Son laboratorios 'móviles'? No
¿Los kits de prueba del suelo se usan comúnmente? NO
14. 11. Fortalezas/debilidades
¿Para qué crees que es fuerte tu laboratorio?
1. Para Investigación
2. Venta de Servicios
3. Recomendaciones de fertilización de cultivos para logar
óptimos rendimientos
4. Recomendaciones para el manejo de la fertilidad de
suelos
¿Qué crees que podría mejorarse?
1. Control de Calidad: Curvas de calibración, curvas de
referencia, preparación de muestras patrón,
2. Fortalecimiento en métodos para análisis físico de
suelos
¿Qué deseas mejorar después de nuestra reunión?
- Fortalecer capacidades en Instrumentalización, control
de calidad , armonización de metodologías, acreditación