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Green and Efficient Extraction and Determination of Melamine in Milk Using Ionic Liquid Dispersive Liquid–Liquid Microextraction

Year: 2026
Type: article
Abstract: ABSTRACT Melamine (2,4,6‐triamino‐1,3,5‐triazine) is a nitrogenous industrial compound, which has been used as an additive in milk and dairy products as a fraudulent means of increasing protein content, and caused several hazardous food contamination episodes around the globe. This study describes a green, inexpensive, and effective methodology based on dispersive liquid–liquid microextraction (DLLME) employing ionic liquid (IL) and subsequent determination of melamine in milk by high‐performance liquid chromatography with photodiode array detector (HPLC‐PDA). Imidazolium‐based IL [C 6 mim][NTf 2 ] was chosen as nontoxic and nonvolatile extraction solvent to substitute toxic and volatile organic solvents usually used in the DLLME process. Extraction parameters such as IL type and volume, disperser solvent type and volume, pH of the sample, ionic strength, extraction time, and centrifugation conditions were optimized using univariate experiments and response surface methodology with Box–Behnken design. With the optimized conditions, the method showed excellent linearity from 0.05 to 5.0 mg kg − 1 ( R 2 ≥ 0.999), limit of detection of 0.015 mg kg − 1 , limit of quantification of 0.045 mg kg − 1 , intra‐ and inter‐day precision (RSD) less than 5%, and spike recoveries of 92.0%–107.0%. The green aspect of the methodology was assessed using AGREE and GAPI indices; both classified this method as environmentally friendly as opposed to traditional liquid–liquid extraction and solid‐phase extraction techniques. The validated method was used to analyze the raw, pasteurized, and powdered milk commercial samples and was found to be within the permitted Codex Alimentarius and local regulatory levels of melamine contamination in dairy products. The IL‐DLLME/HPLC‐PDA approach possesses the advantages of simplicity, high sensitivity, minimal reagent consumption, and environmental friendliness, and thus can be recommended for routine application in food‐safety laboratories.
Language: English
Field: Chemistry
Open Access status: bronze
OpenAlex ID: W7220866505
FWCI:
Cites: 17
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Related to: 10