Determination of Aminoglycosides by Ion-Pair Liquid Chromatography with UV Detection: Application to Pharmaceutical Formulations and Human Serum Samples.

Aminoglycosides (AGs) represent a prominent class of antibiotics widely employed for the treatment of various bacterial infections. Their widespread use has led to the emergence of antibiotic-resistant strains of bacteria, highlighting the need for analytical methods that allow the simple and reliable determination of these drugs in pharmaceutical formulations and biological samples. In this study, a simple, robust and easy-to-use analytical method for the simultaneous determination of five common aminoglycosides was developed with the aim to be widely applicable in routine laboratories.

Changes in vineyard soil parameters after repeated application of organic-inorganic amendments based on spent mushroom substrate.

The changes of physicochemical and biochemical parameters of a silty loam (S1) and sandy loam (S2) vineyard soils added with spent mushroom substrate (SMS) or SMS composted with ophite (OF) as rock dust (SMS + OF) were studied. Two doses of SMS or SMS + OF (25 and 100 Mg ha) were applied for two consecutive years (2020-2021) and changes of soil physicochemical parameters, and dehydrogenase activity (DHA), respiration (RES), microbial biomass (BIO), and the phospholipid fatty acids (PLFAs) profile were assayed on a temporal basis. The results showed an increase in soil organic carbon (OC) content, total and mineralised N, P, and K, especially when the highest SMS dose was applied to soils.

Assessment of pesticide residues in waters and soils of a vineyard region and its temporal evolution.

Sustainable agriculture practices and integrated pest management for avoiding environmental pollution are necessary to maintain a high yield in vineyard areas. Pesticide residues in groundwater in a vineyard area of La Rioja (Spain) have been evaluated in previous years, and they could now have varied after farmers have adopted the different measures recommended. Accordingly, this research's objectives were (i) to evaluate the occurrence and seasonal distribution (spring, summer, and autumn samplings) of pesticides (36) plus their degradation products (DP) (11) in water and soil samples (23 + 15) in La Rioja (Northern Spain), and (ii) to compare the current water quality (2019) with that determined previously (2011).

The role of two organic amendments to modify the environmental fate of S-metolachlor in agricultural soils.

S-metolachlor is a widely used herbicide that may contaminate groundwater when applied to irrigated crops, especially when the soil has a low organic carbon (OC) content. The objective here was to assess the capacity of two organic wastes, namely, green compost (GC) and pelletised organo-mineral manure fertilizer (PM), applied to two soils (S) with different textures at a rate of 10% dry weight to modify the fate of S-metolachlor. The herbicide's Freundlich adsorption coefficient (Kf) increased within a range of 3.

Monitoring and environmental risk assessment of pesticide residues and some of their degradation products in natural waters of the Spanish vineyard region included in the Denomination of Origin Jumilla.

Water pollution by pesticides used in agriculture is currently a major concern both in Spain and in Europe as a whole, prompting the need to evaluate water quality and ecological risk in areas of intensive agriculture. This study involved monitoring pesticide residues and certain degradation products in surface and ground waters of the Denomination of Origin (DO) Jumilla vineyard area in Spain. Sixty-nine pesticides were selected and evaluated at twenty-one sampling points using a multi-residue analytical method, based on solid-phase extraction (SPE) and analysis by liquid chromatography coupled with mass spectrometry (LC-MS), providing reliable results.

Residues of pesticides and some metabolites in dissolved and particulate phase in surface stream water of Cachapoal River basin, central Chile.

In the last twenty years, pesticide use in Chile has increased more than 160%, generating a greater risk of water resources pollution. The objective of this study was to assess the presence of 22 pesticides and 12 degradation products in surface water samples from the Cachapoal River basin, Central Chile, an area characterized by intense agricultural activity. Pesticide concentrations in the dissolved phase (DP) and particulate phase (PP) in samples collected in the dry season and after precipitation events was assessed.

Seasonal distribution of herbicide and insecticide residues in the water resources of the vineyard region of La Rioja (Spain).

Pesticides are needed to maintain high production in the vineyard area of La Rioja (Spain), and monitoring their spatial distribution is a priority for preserving the quality of natural resources. Accordingly, the purpose of this work was to conduct a study to evaluate the presence and seasonal distribution of herbicide and insecticide residues in ground and surface waters in this region. The monitoring network comprised 12 surface waters and 78 groundwaters, covering the three subareas (63,593ha) into which the vineyard region is divided.

Intra-annual trends of fungicide residues in waters from vineyard areas in La Rioja region of northern Spain.

The temporal trends of fungicides in surface and ground water in 90 samples, including both surface waters (12) and ground waters (78) from an extensive vineyard area located in La Rioja (Spain), were examined between September 2010 and September 2011. Fungicides are used in increasing amounts on vines in many countries, and they may reach the water resources. However, few data have been published on fungicides in waters, with herbicides being the most frequently monitored compounds.

Application of mesotrione at different doses in an amended soil: Dissipation and effect on the soil microbial biomass and activity.

The aim of this work was to estimate the dissipation of mesotrione applied at three doses (2, 10 and 50 mg kg(-1) dw) in an unamended agricultural soil, and this same soil amended with two organic residues (green compost (C) and sewage sludge (SS)). The effects of herbicide and organic residue on the abundance and activity of soil microbial communities were also assessed by determining soil microbial parameters such as biomass, dehydrogenase activity (DHA), and respiration. Lower dissipation rates were observed for a higher herbicide dose.

Pesticide residues in vineyard soils from Spain: Spatial and temporal distributions.

Spatial and temporal evaluations of seventeen pesticides and some of their degradation products were carried out in seventeen vineyard soils from La Rioja region (Spain). The soils were sampled in March, June and October 2012, and the pesticides were selected among those previously detected in surface and ground waters from the same area. All pesticides were detected in some of the soils in the three different areas of La Rioja at the different sampling times, with only the metalaxyl metabolite, CGA-62826, not being detected in any of the soils sampled in October.

Development of a procedure for the multiresidue analysis of pesticides in vineyard soils and its application to real samples.

A procedure for multiresidue analysis was developed for the extraction and determination of 17 pesticides, including herbicides, fungicides, and insecticides, as well as certain degradation products, in vineyard soils from La Rioja region (Spain). Different solvents and mixtures were tested in spiked pesticide-free soils, and pesticides were comparatively evaluated by gas chromatography with mass spectrometry and liquid chromatography with mass spectrometry. Recoveries >70%, with relative standard deviations <9%, were obtained when a mixture of methanol/acetone or a mixture of methanol/CaCl2 0.

Effect of different organic amendments on the dissipation of linuron, diazinon and myclobutanil in an agricultural soil incubated for different time periods.

Dissipation kinetics of pesticides belonging to three chemical groups (linuron, diazinon and myclobutanil) was studied in an unamended agricultural soil and in this soil amended with three organic residues: sewage sludge (SS), grape marc (GM) and spent mushroom substrate (SMS). The soils were incubated with the residues outdoors for one and 12 months. Mineralized, extracted and non-extractable fractions were also studied for (14)C-linuron and (14)C-diazinon.

Occurrence of phenols and phenoxyacid herbicides in environmental waters using an imprinted polymer as a selective sorbent.

A monitoring program was developed for the environmental analysis of four phenols and three phenoxyacid herbicides in natural surface and ground water samples from the vineyard region of La Rioja (Spain). An analytical method based on molecularly imprinted solid phase extraction was developed for the determination of the impact of these compounds on the quality of environmental water samples. Different parameters were evaluated and optimized to achieve limits of detection in the 20-90 ng L(-1) range for both surface and ground water, with relative standard deviations in the 12-18% range.

Pesticides and degradation products in groundwaters from a vineyard region: optimization of a multiresidue method based on SPE and GC-MS.

A reliable multiresidue method based on solid phase extraction was developed using GC-MS to determine and quantify 34 pesticides, including herbicides, fungicides, insecticides, and some of their degradation products, in groundwater in a vineyard region of La Rioja (northern Spain). Different parameters were optimized and good recoveries (65-108% range) and precisions (12-19% range) were achieved with spiked water samples for a concentration of 0.1 μg/L.

Long-term variability of metals from fungicides applied in amended young vineyard fields of La Rioja (Spain).

The long-term variability of total Cu content from fungicides applied in a certified wine region of Spain (La Rioja) and of other metals (Cd, Cr, Ni, Pb, and Zn) was evaluated in three young vineyard soils and subsoils unamended and amended with spent mushroom substrates (SMS) over a 3-year period (2006-2008). SMS is a promising agricultural residue as an amendment to increase the soil organic matter content but may modify the behaviour of metals from pesticide utilisation in vineyards. Fresh and composted SMS was applied each year at a rate of 25 t ha(-1) (dry-weight).

Behavior of phenols and phenoxyacids on a bisphenol-A imprinted polymer. Application for selective solid-phase extraction from water and urine samples.

A molecularly imprinted polymer (MIP), obtained by precipitation polymerisation with 4-vinylpyridine as the functional monomer, ethylene glycol dimethacrylate as cross-linker, and bisphenol-A (BPA) as template, was prepared. The binding site configuration of the BPA-MIP was examined using Scatchard analysis. Moreover, the behaviour of the BPA-MIP for the extraction of several phenolic compounds (bisphenol-A, bisphenol-F, 4-nitrophenol, 3-methyl-4-nitrophenol) and phenoxyacid herbicides such as 2,4-D, 2,4,5-T and 2,4,5-TP has been studied in organic and aqueous media in the presence of other pesticides in common use.

Field-scale dissipation of tebuconazole in a vineyard soil amended with spent mushroom substrate and its potential environmental impact.

The persistence, mobility and degradation of tebuconazole were assessed under field conditions in a sandy clay loam soil amended with spent mushroom substrate (SMS) at two rates. The aim was to evaluate the environmental impact of the simultaneous application of SMS and fungicide in a vineyard soil. SMS is the pasteurized and composted organic material remaining after a crop of mushroom is produced.

Automated sample treatment with the injection of large sample volumes for the determination of contaminants and metabolites in urine.

This work reports the development of a simple and automated method for the quantitative determination of several contaminants (triazine, phenylurea, and phenoxyacid herbicides; carbamate insecticides and industrial chemicals) and their metabolites in human urine with a simplified sample treatment. The method is based on the online coupling of an extraction column with RP LC separation-UV detection; this coupling enabled fast online cleanup of the urine samples, efficiently eliminating matrix components and providing appropriate selectivity for the determination of such compounds. The variables affecting the automated method were optimized: sorbent type, washing solvent and time, and the sample volume injected.

[Presence of residues and pollutants in human milk].

The contamination of human milk by xenobiotics is a common problem worldwide which is affected by the geographical, climate-related, cultural and socioeconomic variations in each individual location. Public health policies have dealt with this situation by means of ongoing monitoring and restrictive legislation in order to reduce the damaging effects on the populations and the environment, objectivatable data however being recorded particularly in the developing countries. Overall and individual aspects of waste and contaminating oganochlorines, organophosphorates, antibiotics, polychlorate biphenyls, dioxins and furans, their content values, toxic effects studies and the maximum limits permitted under international legislation are highlighted.

Determination of herbicides and metabolites by solid-phase extraction and liquid chromatography evaluation of pollution due to herbicides in surface and groundwaters.

A procedure based on solid-phase extraction (SPE) has been developed for the simultaneous preconcentration of three widely used herbicides and seven of their most common degradation products. The compounds studied were atrazine and its metabolites, desethylatrazine, desethyldesisopropylatrazine (DEDIA), 2-hydroxyatrazine, desethyl-2-hydroxyatrazine and desisopropyl-2-hydroxyatrazine (DIHA), terbutryne and its metabolite 2-hydroxyterbutylazine, and chlorotoluron and its metabolite 3-chloro-4-methylphenylurea. A HPLC system with diode array detection was used for the separation, identification and quantification of all these analytes.