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2.
P R Health Sci J ; 42(3): 203-206, 2023 09.
Artículo en Inglés | MEDLINE | ID: mdl-37709676

RESUMEN

OBJECTIVE: To evaluate IgG antibody levels against SARS-CoV-2 in non-infected vaccinated subjects among vaccine brand, sex, and age. METHODS: Abbott's AdviseDx SARS-CoV-2 IgG II immunoassay was used to measure IgG levels within 6-9 months after the second dose vaccination; level >50 AU/mL was classified as a positive test. RESULTS: Data of 183 non-infected vaccinated subjects was analyzed according to the vaccine brand, time after second vaccination, sex, and age. Bivariate analysis showed that receiving the Moderna brand vaccine, being female, and younger were associated with higher antibody levels, p<.001. Conversely, no differences were observed between the IgG antibody levels against SARS-CoV-2 and time after second vaccination (6-7 months as compared to 8-9 months), p=.49. CONCLUSION: After six to nine months post-vaccination, receiving the Moderna vaccine, being female, and being younger were significantly associated to higher IgG antibody levels to SARS-CoV-2 in non-infected vaccinated subjects.


Asunto(s)
COVID-19 , Vacunas , Femenino , Humanos , Masculino , COVID-19/prevención & control , SARS-CoV-2 , Vacunación , Inmunoglobulina G
3.
Cir Esp (Engl Ed) ; 101(10): 665-677, 2023 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-37094777

RESUMEN

INTRODUCTION: The effectiveness of the Enhanced Recovery After Surgery (ERAS) protocols in gastric cancer surgery remains controversial. METHODS: Multicentre prospective cohort study of adult patients undergoing surgery for gastric cancer. Adherence with 22 individual components of ERAS pathways were assessed in all patients, regardless of whether they were treated in a self-designed ERAS centre. Each centre had a three-month recruitment period between October 2019 and September 2020. The primary outcome was moderate-to-severe postoperative complications within 30 days after surgery. Secondary outcomes were overall postoperative complications, adherence to the ERAS pathway, 30 day-mortality and hospital length of stay (LOS). RESULTS: A total of 743 patients in 72 Spanish hospitals were included, 211 of them (28.4 %) from self-declared ERAS centres. A total of 245 patients (33 %) experienced postoperative complications, graded as moderate-to-severe complications in 172 patients (23.1 %). There were no differences in the incidence of moderate-to-severe complications (22.3% vs. 23.5%; OR, 0.92 (95% CI, 0.59 to 1.41); P = 0.068), or overall postoperative complications between the self-declared ERAS and non-ERAS groups (33.6% vs. 32.7%; OR, 1.05 (95 % CI, 0.70 to 1.56); P = 0.825). The overall rate of adherence to the ERAS pathway was 52% [IQR 45 to 60]. There were no differences in postoperative outcomes between higher (Q1, > 60 %) and lower (Q4, ≤ 45 %) ERAS adherence quartiles. CONCLUSIONS: Neither the partial application of perioperative ERAS measures nor treatment in self-designated ERAS centres improved postoperative outcomes in patients undergoing gastric surgery for cancer. TRIAL REGISTRATION: ClinicalTrials.gov Identifier NCT03865810.


Asunto(s)
Recuperación Mejorada Después de la Cirugía , Neoplasias Gástricas , Adulto , Humanos , Atención Perioperativa , Complicaciones Posoperatorias/epidemiología , Complicaciones Posoperatorias/etiología , Estudios Prospectivos , Neoplasias Gástricas/cirugía , Neoplasias Gástricas/complicaciones
5.
Foods ; 11(24)2022 Dec 12.
Artículo en Inglés | MEDLINE | ID: mdl-36553756

RESUMEN

The consumption of bee pollen has increased in the last few years due to its nutritional and health-promoting properties, which are directly related to its bioactive constituents, such as amino acids. Currently, there is great interest in understanding the role of these in bee products as it provides relevant information, e.g., regarding nutritional value or geographical and botanical origins. In the present study, two fast chromatographic methods were adapted based on commercial EZ:faast™ kits for gas chromatography-mass spectrometry and liquid chromatography−mass spectrometry for determining free amino acids in bee pollen. Both methods involved the extraction of amino acids with water, followed by a solid phase extraction to eliminate interfering compounds, and a derivatization of the amino acids prior to their chromatographic separation. The best results in terms of run time (<7 min), matrix effect, and limits of quantification (3−75 mg/kg) were obtained when gas chromatography−mass spectrometry was employed. This latter methodology was applied to analyze several bee pollen samples obtained from local markets and experimental apiaries. The findings obtained from a statistical examination based on principal component analysis showed that bee pollen samples from commercial or experimental apiaries were different in their amino acid composition.

6.
Food Res Int ; 160: 111698, 2022 10.
Artículo en Inglés | MEDLINE | ID: mdl-36076401

RESUMEN

In the last years, an increase has been observed in the adulteration of bee pollen. Consequently, different tools are required to authenticate the origin of this product, such as a study of the profile and composition of a specific family of compounds. The present study investigates the potential of betaines and related compounds as markers of the apiary of origin and harvest period of 71 bee pollen samples. These were collected from four apiaries (Pistacho, Tío Natalio, Monte and Fuentelahiguera), located in the same geographical area (Guadalajara, Spain) and sampled during three consecutive harvest periods in the same year (April-May, June, July-August). They were analyzed by means of a previously developed methodology, which involved solvent extraction, hydrophilic interaction liquid chromatography coupled to mass spectrometry, and a statistical analysis of the data (canonical discriminant analysis). Variable amounts of betaines and related compounds were found in the samples, with four of these being identified in all of them (betonicine, betaine, trigonelline and choline); betonicine was the predominant compound in a concentration range of 264 to 52384 mg/kg. It was possible to statistically assign over 50 % of the samples to the corresponding apiary of origin, the best results being obtained for the Tío Natalio apiary (75 %); this classification was even better in the case of the harvest period, as more than 75 % of the samples were correctly assigned, and in two periods (April-May and June) a 90 % rate was obtained.


Asunto(s)
Compuestos de Amonio , Betaína , Animales , Abejas , Betaína/análisis , Cromatografía Liquida , Análisis Discriminante , Polen/química
7.
Food Res Int ; 130: 108904, 2020 04.
Artículo en Inglés | MEDLINE | ID: mdl-32156359

RESUMEN

The objective of this study was to propose a novel method to determine residues of the bio-insecticide spinetoram, which is a mixture of two components (spinetoram J and L), in honey from multifloral, rosemary and heather botanical origins; liquid chromatography coupled to quadrupole time-of-flight mass spectrometry was the technique employed. An efficient sample treatment (recoveries between 82% and 95%) involving a solid-phase extraction with a polymeric sorbent has been recommended, and no matrix effect was observed. Chromatographic analysis (4 min) was performed in reverse phase mode by using a fused-core column (Kinetex® EVO C18) with acetonitrile and ammonium formate as the mobile phase components, which was applied in isocratic elution mode. Method was validated according to the current European legislation. Not only was it selective, but it also displayed a wide linear range, good precision (relative standard deviation values lower than 9%) and sensitivity (low limits of detection (spinetoram J, 0.1-0.3 µg/kg; spinetoram L, 0.1-0.2 µg/kg) and quantification (spinetoram J, 0.3-1.2 µg/kg; spinetoram L, 0.4-0.7 µg/kg)). Several honey samples were analyzed with this method and no spinetoram residues were found above the limits of detection.


Asunto(s)
Cromatografía Liquida/métodos , Miel/análisis , Macrólidos/análisis , Extracción en Fase Sólida/métodos , Espectrometría de Masas en Tándem/métodos , Reproducibilidad de los Resultados
10.
Cardiovasc Revasc Med ; 19(5 Pt A): 493-497, 2018 07.
Artículo en Inglés | MEDLINE | ID: mdl-29169982

RESUMEN

AIMS: To analyse systematic isolated post-dilatation of the side branch as a part of provisional stent technique. METHODS: 1960 angioplasties performed in two centres were prospectively registered, of which 382 were coronary bifurcations with a side branch>2mm. In centre A, isolated post-dilatation of the side branch was performed regardless its impairment after main vessel stenting. In centre B, side branch post-dilatation was performed only if it was severely affected after stent implantation. RESULTS: There was no difference between the two centres in the rate of side branch affection after stent implantation (A: 44.6 vs B: 49.3%, p=0.48) nor in the procedural success rate (A: 98.6% vs B: 96.7%, p=0.45). After one-year follow-up, a reduction of cardiovascular events was observed in centre A (A: 4.4% vs B: 10.4%, p=0.043) with a trend towards lower cardiac mortality (A: 2.2% vs B: 6.5%, p=0.093) and stent thrombosis (A: 0% vs B: 2.6%, p=0.077). There were no differences in the rate of myocardial infarction related to the treated artery (A: 1.4% vs B: 3.9%, p=0.29), or target lesion revascularization (A: 1.4% vs. B: 3.2%, p=0.45). CONCLUSIONS: Systematic isolated post-dilatation of the side branch in the provisional stent technique was associated with a high angiographic success rate, and a low rate of cardiovascular events during follow-up. Although the study design does not allow definitive conclusions, this strategy could be considered a valid option in some cases or even as part of the provisional stent technique.


Asunto(s)
Angioplastia Coronaria con Balón/instrumentación , Enfermedad de la Arteria Coronaria/cirugía , Stents , Anciano , Angioplastia Coronaria con Balón/efectos adversos , Angioplastia Coronaria con Balón/mortalidad , Angiografía Coronaria , Enfermedad de la Arteria Coronaria/diagnóstico por imagen , Enfermedad de la Arteria Coronaria/mortalidad , Trombosis Coronaria/diagnóstico por imagen , Trombosis Coronaria/etiología , Femenino , Humanos , Masculino , Persona de Mediana Edad , Estudios Prospectivos , Radiografía Intervencional , Sistema de Registros , Factores de Riesgo , España , Factores de Tiempo , Resultado del Tratamiento
12.
Minerva Chir ; 72(1): 10-17, 2017 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-27787484

RESUMEN

BACKGROUND: The aim of this study was to describe the trends in surgical routes in obese women who underwent hysterectomy for benign disease at our center and compare complications in different groups. METHODS: Retrospective study done between 2011 and 2015 in women with a Body Mass Index≥30 who underwent hysterectomy for benign disease at Virgen de las Nieves Universitary Hospital in Granada, Spain. We studied three groups based on the surgical route chosen for hysterectomy: vaginal, abdominal or laparoscopic. The rates of intraoperative and postoperative complications, major complications, reintervention and days of hospital stay were compared. RESULTS: Abdominal hysterectomy was associated with the highest risk of postoperative complications and the longest hospital stay. Laparoscopic hysterectomy had a higher risk than vaginal hysterectomy of major complications. There were no significant differences between groups for any of the other variables. CONCLUSIONS: In obese women vaginal hysterectomy was associated with the lowest morbidity, and should be the approach of choice whenever feasible.


Asunto(s)
Histerectomía/métodos , Laparoscopía , Obesidad/cirugía , Enfermedades Uterinas/cirugía , Anciano , Índice de Masa Corporal , Femenino , Estudios de Seguimiento , Humanos , Histerectomía Vaginal/métodos , Tiempo de Internación , Persona de Mediana Edad , Obesidad/complicaciones , Estudios Retrospectivos , Factores de Riesgo , Resultado del Tratamiento , Enfermedades Uterinas/complicaciones
13.
Rev. esp. cardiol. (Ed. impr.) ; 69(4): 377-383, abr. 2016. ilus, graf, tab
Artículo en Español | IBECS | ID: ibc-152028

RESUMEN

Introducción y objetivos: El papel de la estimulación auriculoventricular secuencial en pacientes con miocardiopatía hipertrófica obstructiva y síntomas incapacitantes sigue siendo controvertido. El objetivo de este trabajo es valorar su efecto en los síntomas, el gradiente dinámico y la función del ventrículo izquierdo. Métodos: Desde 1991 a 2009, se implantó un marcapasos bicameral a 82 pacientes con miocardiopatía hipertrófica obstructiva y síntomas incapacitantes a pesar de tratamiento médico óptimo. Se programó una estimulación secuencial con un intervalo auriculoventricular corto. Se analizaron parámetros clínicos y ecocardiográficos antes, inmediatamente tras el implante y al final de un largo seguimiento (mediana, 8,5 [1-18] años). Resultados: La clase funcional de la New York Heart Association se redujo inmediatamente tras el implante en el 95% de los pacientes (p < 0,0001), y esta mejoría se mantenía al final del seguimiento en el 89% (p = 0,016). Se observó una reducción significativa del gradiente tras el implante (94,5 ± 36,5 frente a 46,4 ± 26,7 mmHg; p < 0,0001) y al final del seguimiento (94,5 ± 36,5 frente a 35,9 ± 24,0 mmHg; p < 0,0001). La insuficiencia mitral mejoró de manera constante en el 52% de los casos (p < 0,0001). No hubo diferencias en el grosor o los diámetros ventriculares, la fracción de eyección o la función diastólica. Conclusiones: La estimulación secuencial en pacientes seleccionados con miocardiopatía hipertrófica obstructiva mejora la clase funcional y reduce el gradiente dinámico y la insuficiencia mitral inmediatamente tras el implante y al final de un largo seguimiento. La estimulación ventricular prolongada no produce efectos deletéreos en la función ventricular sistólica o diastólica en estos pacientes (AU)


Introduction and objectives: Controversy persists regarding the role of sequential atrioventricular pacing in patients with obstructive hypertrophic cardiomyopathy and disabling symptoms. The aim of this study was to evaluate the effect of pacing on symptoms, dynamic gradient, and left ventricular function in patients with hypertrophic cardiomyopathy. Methods: From 1991 to 2009, dual-chamber pacemakers were implanted in 82 patients with obstructive hypertrophic cardiomyopathy and disabling symptoms despite optimal medical therapy. Sequential pacing was performed with a short atrioventricular delay. Clinical and echocardiographic parameters were measured before and immediately after implantation and after a long follow-up (median, 8.5 years [range, 1-18 years]). Results: The New York Heart Association functional class was immediately reduced after pacemaker implantation in 95% of patients (P < .0001), and this improvement was maintained until the final follow-up in 89% (P = .016). The gradient was significantly reduced after implantation (94.5 ± 36.5 vs 46.4 ± 26.7 mmHg; P < .0001) and at final follow-up (94.5 ± 36.5 vs 35.9 ± 24.0 mmHg; P < .0001). Mitral regurgitation permanently improved in 52% of the patients (P < .0001). There were no differences in ventricular thickness or diameters, ejection fraction, or diastolic function. Conclusions: Sequential pacing in selected patients with obstructive hypertrophic cardiomyopathy improves functional class and reduces dynamic gradient and mitral regurgitation immediately after pacemaker implantation and at final follow-up. Prolonged ventricular pacing has no negative effects on systolic or diastolic function in these patients (AU)


Asunto(s)
Humanos , Estimulación Cardíaca Artificial/métodos , Cardiomiopatía Hipertrófica/terapia , Marcapaso Artificial , Cardiomiopatía Hipertrófica/fisiopatología , Insuficiencia de la Válvula Mitral/prevención & control , Obstrucción del Flujo Ventricular Externo/fisiopatología , Estimulación Cardíaca Artificial
14.
Rev Esp Cardiol (Engl Ed) ; 69(4): 377-83, 2016 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-26719031

RESUMEN

INTRODUCTION AND OBJECTIVES: Controversy persists regarding the role of sequential atrioventricular pacing in patients with obstructive hypertrophic cardiomyopathy and disabling symptoms. The aim of this study was to evaluate the effect of pacing on symptoms, dynamic gradient, and left ventricular function in patients with hypertrophic cardiomyopathy. METHODS: From 1991 to 2009, dual-chamber pacemakers were implanted in 82 patients with obstructive hypertrophic cardiomyopathy and disabling symptoms despite optimal medical therapy. Sequential pacing was performed with a short atrioventricular delay. Clinical and echocardiographic parameters were measured before and immediately after implantation and after a long follow-up (median, 8.5 years [range, 1-18 years]). RESULTS: The New York Heart Association functional class was immediately reduced after pacemaker implantation in 95% of patients (P < .0001), and this improvement was maintained until the final follow-up in 89% (P = .016). The gradient was significantly reduced after implantation (94.5 ± 36.5 vs 46.4 ± 26.7mmHg; P < .0001) and at final follow-up (94.5 ± 36.5 vs 35.9 ± 24.0mmHg; P < .0001). Mitral regurgitation permanently improved in 52% of the patients (P < .0001). There were no differences in ventricular thickness or diameters, ejection fraction, or diastolic function. CONCLUSIONS: Sequential pacing in selected patients with obstructive hypertrophic cardiomyopathy improves functional class and reduces dynamic gradient and mitral regurgitation immediately after pacemaker implantation and at final follow-up. Prolonged ventricular pacing has no negative effects on systolic or diastolic function in these patients.


Asunto(s)
Estimulación Cardíaca Artificial , Cardiomiopatía Hipertrófica/terapia , Predicción , Función Ventricular Izquierda/fisiología , Obstrucción del Flujo Ventricular Externo/terapia , Adulto , Anciano , Anciano de 80 o más Años , Cardiomiopatía Hipertrófica/complicaciones , Cardiomiopatía Hipertrófica/diagnóstico , Ecocardiografía , Femenino , Estudios de Seguimiento , Ventrículos Cardíacos/diagnóstico por imagen , Ventrículos Cardíacos/fisiopatología , Humanos , Masculino , Persona de Mediana Edad , Estudios Retrospectivos , Resultado del Tratamiento , Obstrucción del Flujo Ventricular Externo/etiología , Obstrucción del Flujo Ventricular Externo/fisiopatología , Adulto Joven
15.
J Chromatogr A ; 1428: 220-7, 2016 Jan 08.
Artículo en Inglés | MEDLINE | ID: mdl-26545338

RESUMEN

A study was carried out to evaluate the possible presence of thiamethoxam, clothianidin and imidacloprid, as well as the metabolic breakdown products of these three neonicotinoids in pollen and honey obtained from brood chamber combs of honeybee colonies located next to sunflower and maize crops from coated seeds. Samples were analyzed by liquid chromatography coupled to quadrupole-time-of-flight mass spectrometry detector, in combination with accurate mass tools such as diagnostic ions by exact mass, chlorine mass filters, and MS/MS experiments. The presence of thiamethoxam and clothianidin was confirmed in some of the pollen samples analyzed. Moreover, different metabolites of neonicotinoids were tentatively detected in the pollen and honey samples collected. The results suggested that four metabolites were found in the honey samples, while for pollen samples eleven metabolites were identified; among these, five were considered for the first time as metabolic breakdown products in sunflower and maize plants.


Asunto(s)
Técnicas de Química Analítica/métodos , Productos Agrícolas/química , Guanidinas/análisis , Miel/análisis , Imidazoles/análisis , Nitrocompuestos/análisis , Oxazinas/análisis , Polen/química , Tiazoles/análisis , Animales , Cromatografía Liquida , Guanidinas/metabolismo , Helianthus/química , Imidazoles/metabolismo , Neonicotinoides , Nitrocompuestos/metabolismo , Oxazinas/metabolismo , Reproducibilidad de los Resultados , Semillas/química , Espectrometría de Masas en Tándem , Tiametoxam , Tiazoles/metabolismo , Zea mays/química
16.
Artículo en Inglés | MEDLINE | ID: mdl-26678670

RESUMEN

A validated analytical method to determine seven neonicotinoids (dinotefuran, nitenpyram, thiamethoxam, clothianidin, imidacloprid, acetamiprid and thiacloprid) in sunflower seeds (hull and kernel) using HPLC coupled to electrospray ionisation mass spectrometry (ESI-MS) is presented. Sample clean-up based on a solid-liquid extraction, and the removal of lipid fraction, in the case of kernels, is proposed and optimised. Low limits of detection and quantification were obtained, ranging from 0.3 × 10(-3) to 1.2 × 10(-3) µg g(-1) and from 1.0 × 10(-3) to 4.0 × 10(-3) µg g(-1), with good precision, and recovery values ranged from 90% to 104% for hulls and kernels. The method was applied for the analysis of five thiamethoxam-dressed sunflower seeds and four non-treated seeds, where, besides thiamethoxam, residues of the other neonicotinoid, clothianidin, were also detected and confirmed via tandem mass spectrometry (LC-ESI-MS/MS). Finally, the presence of residues of thiamethoxam and clothianidin in collected sunflower seeds (hulls) coming from coated seeds confirmed the translocation of these neonicotinoids through the plant up to these seeds.


Asunto(s)
Helianthus/química , Insecticidas/análisis , Insecticidas/química , Residuos de Plaguicidas/análisis , Semillas/química , Cromatografía Líquida de Alta Presión , Guanidinas/análisis , Imidazoles/análisis , Neonicotinoides , Nitrocompuestos/análisis , Oxazinas/análisis , Piridinas/análisis , Espectrometría de Masas en Tándem , Tiametoxam , Tiazinas/análisis , Tiazoles/análisis
17.
J Chromatogr A ; 1359: 317-24, 2014 Sep 12.
Artículo en Inglés | MEDLINE | ID: mdl-25085817

RESUMEN

This paper represents the first report of a capillary electrophoresis (CE) method compatible with mass spectrometry (MS) detection for simultaneously analyzing seven neonicotinoid insecticides (acetamiprid, clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid and thiamethoxam). Different variables affecting CE separation (buffer concentration, pH, applied voltage and injection time) and MS detection (electrospray parameters) were studied. Low limits of detection (LOD) and quantification (LOQ) were achieved for all analytes, ranging from 1.0 to 2.3µg/L, and from 3.5 to 7.2µg/L, respectively. In addition, the proposed method showed itself to be linear in the range from LOQ to 1000µg/L and to be precise, as the relative standard deviations of the migration times were lower than 4% in all cases. Finally, the proposed CE-MS method was applied to assess the efficacy of a beeswax cleaning treatment with oxalic acid to remove residues of three of the most commonly used neonicotinoids (clothianidin, imidacloprid and thiamethoxam), use of which has recently been restricted by the European Union.


Asunto(s)
Electroforesis Capilar/métodos , Insecticidas/análisis , Espectrometría de Masas en Tándem/métodos , Guanidinas/análisis , Imidazoles/análisis , Límite de Detección , Espectrometría de Masas , Neonicotinoides , Nitrocompuestos/análisis , Oxazinas/análisis , Piridinas/análisis , Tiametoxam , Tiazinas/análisis , Tiazoles/análisis , Ceras/análisis
18.
J Sep Sci ; 37(3): 204-10, 2014 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-24243865

RESUMEN

This paper reports the use of a new LC method with a fused-core analytical column coupled to ESI-MS to determine residues of the biopesticide spinosad in bee pollen and beeswax. The method analyzes the active ingredients, spinosyns A and D, with a simple and efficient sample treatment (recovery between 90 and 105%) consisting of a solid-liquid extraction with acetone (bee pollen) or acetonitrile (beeswax). The method was validated in terms of selectivity, LOD, LOQ, linearity, and precision. The LOD and LOQ values ranged between 0.1-0.2 and 0.4-0.7 µg/kg, respectively. Moreover, the precision obtained within the linear concentration range (LOQ 500 µg/kg) was satisfactory (RSD lower than 5%). Finally, the proposed method was applied to analyze bee pollen and beeswax samples collected from apiaries located close to fruit orchards in two Spanish regions.


Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Macrólidos/análisis , Residuos de Plaguicidas/análisis , Polen/química , Espectrometría de Masa por Ionización de Electrospray/métodos , Espectrometría de Masas en Tándem/métodos , Ceras/análisis , Animales , Combinación de Medicamentos , Macrólidos/aislamiento & purificación , Residuos de Plaguicidas/aislamiento & purificación , Extracción en Fase Sólida
19.
J Chromatogr A ; 1313: 24-36, 2013 Oct 25.
Artículo en Inglés | MEDLINE | ID: mdl-23891212

RESUMEN

In the last years, supercritical fluid chromatography (SFC) has increased its acceptance between scientists. The unique selectivity, short analysis times, low consumption of organic solvents as well as the improvements in instrumentation have contributed to expand its use. These characteristics make SFC a powerful tool when food analysis requires individualized evaluation of several compounds in very complex samples. In this work, the advantages and main applications of SFC in food analysis are reviewed, focusing special attention onto analytical and preparative separations.


Asunto(s)
Cromatografía con Fluido Supercrítico/métodos , Análisis de los Alimentos/métodos , Carotenoides/análisis , Lípidos/análisis
20.
J Sep Sci ; 36(16): 2593-601, 2013 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-23733735

RESUMEN

A new and sensitive analytical method is presented to determine nine anticoagulant rodenticide (chlorophacinone, bromadiolone, pindone, diphacinone, warfarin, coumatetralyl, brodifacoum, floucomafen, and difenacoum) residues in water and soil samples by LC-ESI-MS. Rodenticides were extracted from soil using a methanol and ammonium formate 30 mM mixture, while ethyl acetate was employed in the water samples. A Gemini 5 µm C18 column was employed, and a mobile phase comprising a mixture of ammonium formate 30 mM and di-n-butylamine 30 mM in water (pH 3.5), ammonium formate 30 mM and di-n-butylamine 20 mM in water (pH 4.4), ammonium formate 30 mM in water (pH 6.5), and methanol in a gradient elution mode was selected. The method was fully validated and it was found to be selective and precise in terms of linearity and accuracy. Extraction recoveries ranged from 90 to 104% for the compounds studied, while the detection and quantification limits were between 0.09 and 2.2 µg/kg in soil or 0.08 and 1.7 µg/L in water. The method was applied to simultaneously measure these compounds in water and soil samples.


Asunto(s)
Anticoagulantes/química , Cromatografía Líquida de Alta Presión/métodos , Rodenticidas/química , Contaminantes del Suelo/química , Espectrometría de Masa por Ionización de Electrospray/métodos , Contaminantes Químicos del Agua/química , Estructura Molecular
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