Development of an ASE‐GC‐MS/MS method for detecting dinitolmide and its metabolite 3‐ANOT in eggs

Abstract

An accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry (ASE-GC-MS/MS) method for detecting dinitolmide residue and its metabolite (3-amino-2-methyl-5-nitrobenzamide, 3-ANOT) in eggs was developed and optimized. The samples were extracted using ASE with acetonitrile as the extractant and were purified by passage through a neutral alumina solid-phase extraction column. Then, the samples were analyzed using the GC-MS/MS method. The optimized method parameters were validated according to the requirements set forth by the European Union and the Food and Drug Administration. The average recoveries of dinitolmide and 3-ANOT from eggs (egg white, egg yolk, and whole egg) at the limit of quantification (LOQ), 0.5 maximum residue limit (MRL), 1 MRL, and 2 MRL were 82.74% to 87.49%, the relative standard deviations (RSDs) were less than 4.63%, and the intra-day RSDs and the inter-day RSDs were 2.96% to 5.21% and 3.94% to 6.34%, respectively. The limits of detection and the LOQ were 0.8 to 2.8 μg/kg and 3.0 to 10.0 μg/kg, respectively. The decision limits (CC ) were 3001.69 to 3006.48 μg/kg, and the detection capabilities (CC ) were 3001.74 to 3005.22 μg/kg. Finally, the new method was successfully applied to the quantitative determination of dinitolmide and 3-ANOT in 50 commercial eggs from local supermarkets.

Comprehensive Strategy for Sample Preparation for the Analysis of Food Contaminants and Residues by GC–MS/MS: A Review of Recent Research Trends

“…In order to achieve a practical and reliable method, several preparation methods have been developed. Extraction by a solvent is the classic sample preparation technique, which includes liquid-liquid extraction (LLE), soxhlet extraction, solid-liquid extraction (SLE), microwave-assisted extraction (MAE), ultrasonic extraction (USE), accelerated solvent extraction (ASE), and supercritical fluid extraction (SFE) [14][15][16][17][18][19][20][21][22]. Improved extraction methods, such as pressurized liquid extraction (PLE), can increase the diffusion rate and solubility of interferences into the matrix [23,24].…”

Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass Spectrometry

“…Several solvents were tested, including acetone, n-hexane, dichlormethane and n-hexane and acetone (1:1 v/v) mixture. After static extraction, the extraction cell was purged with nitrogen for 1 min [24]. The extracts were collected in 240 mL collection bottles and concentrated to about 5 mL with a rotary evaporator, then evaporated at 50 • C to dry.…”

“…Drying and homogenization followed by accelerate solvent extraction using a low polarity solvent has proven to be an efficient, reproducible and simple extractive method for acetochlor and s-metolachlor. Various solvents such as pure n-hexane, acetonitrile and a mixture of acetone and DCM, DCM and ethylacetate have been used for the ASE of anilide herbicides [17,24,25]. The best extraction efficiency requires selection of an appropriate solvent which has similar polarity with target analytes [26,27].…”