Fungicides In Samples Research Articles

Determination of Azole Fungicide Residues in Fresh Juice by Magnetic Solid Phase Extraction Based on Fe3O4@ZnAl-LDH@MIL-53(Al) Sorbent in Combination with High-Performance Liquid Chromatograph.

In this work, a magnetic adsorption material based on metal-organic framework (Fe3O4@ZnAl-LDH@MIL-53(Al)) was synthesized and used as an adsorbent in the process of magnetic solid phase extraction. Then, a high-performance liquid chromatograph was used to quantitatively detect triazole fungicides in samples. In order to verify the successful preparation of the material, a series of characterization analyses were carried out. Besides, the key parameters that may affect the extraction efficiency have been optimized, and under optimal conditions the three triazole fungicides showed good linearity in the range of 10-1000μg/L (R2 ≥ 0.9796); Limit of detections were ranged from 0.013 to 0.030μg/mL. Finally, the established method was applied to the detection of triazole fungicides in four fresh juice samples. The results showed that the target analyte was not detected in all the test samples. By detecting the recoveries (73.3-104.3%) and coefficient variation (RSD ≤ 6.8%) of triazole fungicides in fortified samples, it proved that this established method meets the requirements of pesticide residue analysis and showed excellent application potential.

A simple co-precipitation sorbent-based preconcentration method for the analysis of fungicides in water and juice samples by high-performance liquid chromatography coupled with photodiode array detection

A magnesium hydroxide co-precipitation sorbent-based method in the presence of an anionic surfactant (e.g., sodium dodecylbenzenesulfonate) and high-performance liquid chromatography were used to preconcentrate and analyze fungicides in water and apple juice samples. The preconcentration procedure can be accomplished in a single step based on the co-precipitation of target fungicides and magnesium chloride in the presence of surfactant in a sodium hydroxide solution (pH 11) and a white precipitate gel was simply obtained after centrifugation. The property of precipitate phase was subsequently characterized using Fourier-transform infrared spectroscopy, scanning electron microscopy, and X-ray diffractometry. Under the optimum conditions, the developed method exhibited good sensitivity, with an enrichment factor of 11–18 and limits of detection of approximately 1–5 μg/L for water samples and 7–10 μg/L for apple juices. High reproducibility was achieved with a relative standard deviation of less than 11%, and a good recovery range of 72% to 120% was also obtained. The proposed method was shown to be a simple preconcentration procedure for concentrating fungicides in the samples investigated.

Target and Nontarget Screening of Organic Micropollutants in Water by Solid-Phase Microextraction Combined with Gas Chromatography/High-Resolution Time-of-Flight Mass Spectrometry

The potential of gas chromatography coupled to high-resolution time-of-flight mass spectrometry (GC/TOF-MS) for screening of organic pollutants in water has been explored. After optimization of the solid-phase microextraction (SPME) step, where parameters such as fiber selection and addition of salt were studied, this extraction technique was applied to the analysis of different types of water samples. Investigation of 60 target organic pollutants, including pesticides, octyl/nonyl phenols, pentachlorobenzene, and polycyclic aromatic hydrocarbons (PAHs) was carried out by evaluating the presence of up to five representative m/z ions per analyte, measured at high mass accuracy, and the attainment of their Q/q (Q, quantitative ion; q, confirmative ion) intensity ratio. This strategy led to the detection of 4-t-octylphenol, simazine, terbuthylazine, chlorpyrifos, terbumeton, and terbutryn in several water samples at low part-per-billion levels. Full spectrum acquisition data generated by the TOF-MS analyzer also allowed subsequent investigation of the presence of polybrominated diphenyl ethers and several fungicides in samples after MS data acquisition, without the need to reanalyze the water samples. In addition, nontarget analysis was also tested by application of a deconvolution software. Several organic pollutants that did not form a part of the list of contaminants investigated were identified in the water samples, thanks to the excellent sensitivity of TOF-MS in full spectrum acquisition mode and the valuable accurate mass information provided by instrument. Bisphenol A, the antioxidant 3,5-di-tert-butyl-4-hydroxy-toluene (BHT), its metabolite 3,5-di-tert-butyl-4-hydroxybenzaldehyde (BHT-CHO), the polycyclic musk galaxolide, and the UV filter benzophenone were some of the compounds present in the water samples analyzed. SPME in combination with GC/TOF-MS has been proved to be an attractive and powerful approach for the rapid screening of multiclass organic pollutants in water, with very little sample manipulation and no solvent consumption. This combination provides to the analyst with information-rich MS data that facilitates the reliable identification of many different organic compounds in samples.