Quantification of pendimethalin in soil and garlic samples by microwave-assisted solvent extraction and HPLC method

A method for the residual pendimethalin in soil and vegetable samples was developed. The method is based on extraction of pendimethalin from samples using microwave-assisted solvent extraction (MASE) with acetone, ethanol, and water as extraction solvent. Extracted pendimethalin samples were analyzed by high-performance liquid chromatography with ultraviolet detector at 240 nm. The MASE parameters, temperature, heating time, and solvent types were optimized with the feasibility of MASE application in the determination of pendimethalin extraction efficiency of pendimethalin from soil and vegetable samples. The maximum temperature that can be used during the heating for MASE is 60°C, where the recovery percentages reached 97%. Linearity for pendimethalin was found in the range of 2?C20 ??g mL^???1 with limits of detection and limits of quantification of 0.059 and 0.17 ??g mL^???1, respectively.     

Determination of ametryn in sugarcane and ametryn–atrazine herbicide formulations using spectrophotometric method

A sensitive spectrophotometric method has been developed for determination of ametryn in agricultural samples. The proposed method was based on reaction with pyridine and further coupling with sulfanilic acid to form a colored product. The absorbance was measured at 400 nm with a molar absorptivity of 2.1 × 10⁵ L mol⁻¹ cm⁻¹. The method shows a linear range from 0.2–20 μg mL⁻¹ with limit of detection and limit of quantification 0.16 and 0.54 μg mL⁻¹, respectively. The method has been successfully applied to the determination of ametryn in sugarcane juice and commercial formulations after separation of ametryn from triazine herbicides based on solvent extraction. Recovery values were found to be in the range of 96.0 ± 0.2% to 98.4 ± 0.1%.     

Spectrophotometric determination of trifluralin in commercial formulations and agricultural samples using factorial design

A simple spectrophotometric method was developed for determination of trifluralin in commercial formulation and food samples. The method was based on the hydrolysis of trifluralin with sodium hydroxide to form 2,6-dinitro-4-trifluoromethylaniline. The resultant aniline group was diazotized with nitrate in acidic media and the diazotized product was coupled with β-naphthol to form red colored product having λ_max 550 nm. The reaction conditions were optimized for hydrolysis as well as for the diazotization reaction. The Beer’s law was obeyed over the range of 0.2–17 μg mL⁻¹ with molar absorptivity of 1.5 × 10⁴ L mol⁻¹ cm⁻¹. The relative standard deviation was found to be 3.6%. A two level factorial design of 2³ was used for optimization of all parameters. The influence of different factors and their interactions on the final azo dye formation were also studied from these factorial designs. The method has been applied successfully for the analysis of commercial formulations and agricultural samples. The recovery for the determination of trifluralin was found to be in the range 95–97%.     

Quantification of triazine herbicides in soil by microwave-assisted extraction and high-performance liquid chromatography

A method for the determination of herbicides residues, triazine (atrazine, metribuzin, ametryn, and terbutryn), in soil samples with high-performance liquid chromatography (HPLC)?CUV detection is described. The proposed method is based on microwave-assisted extraction (MAE) of soil samples for 4 min at 80% of 850-W magnetron outputs in the presence of mixture of solvents (methanol/acetonitrile/ethylacetate). Related important factors influencing the MAE efficiency, such as the solvent type and volume, irradiation energy, and time, were optimized in detail. Calibration curve ranges established using HPLC for metribuzin, atrazine, ametryn, and terbutryn are 1.0?C19.0, 0.9?C18.0, 0.6?C11.0, and 0.7?C11.0 µg mL^???1, respectively. The limits of detection of metribuzin, atrazine, ametryn, and terbutryn are 0.30, 0.24, 0.16, and 0.20 µg mL^???1 while limits of quantification are 1.0, 0.80, 0.50, and 0.60 µg mL^???1, respectively. A Plackett?CBurman factorial design was used as a screening method in order to select the variables that influence MAE extraction. The recoveries of the method at three different spiked levels were assessed by analyzing real soil samples and were found to be in the range of 83.33 ± 0.12?C96.33 ± 0.23 with good precision (<8%).     

Development of a complex-based flow injection spectrophotometric method for determination of the herbicide pinoxaden in environmental samples

A flow injection (FI) spectrophotometric method for the determination of the herbicide pinoxaden (PXD) has been proposed. PXD was converted in alkaline media with hydroxylamine hydrochloride to the hydroxamate salt. The salt was reacted with iron(III) chloride, and the absorbance of the red colored tris iron hydroxamate complex was measured at 500?nm using a FI system. The method was found to be linear between 0.5 and 40?mg?L^?1 with a molar absorptivity of 1.53?×?10^4?L?mol^?1?cm^?1. The limit of detection and limit of quantification were found to be 0.1?±?0.01?mg?L^?1 and 0.6?±?0.05?mg?L^?1, respectively. Any interference of fenoxaprop-p-ethyl (FE) was avoided by the separation of PXD by liquid chromatography with a mixture of dichloromethane and n-hexane (1?:?1) as eluent. The method was applied to the determination of PXD in soil, water, and wheat grains with percent recoveries of 98?±?2, 100?±?2, and 98?±?5, respectively. Sample throughput of 60 samples per hour was achieved under optimized conditions.