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Quantification of Melamine in Milk and Dairy Products by Liquid Chromatography after a Simple Sample Clean‐Up Procedure
Author(s) -
Elsheikh Amjad H.,
Aldegs Yahya S.,
AbuWardeh Asma'a H.,
Alghouti Mohammad A.
Publication year - 2017
Publication title -
journal of food processing and preservation
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.511
H-Index - 48
eISSN - 1745-4549
pISSN - 0145-8892
DOI - 10.1111/jfpp.12867
Subject(s) - melamine , chromatography , chemistry , extraction (chemistry) , sonication , centrifugation , filtration (mathematics) , infant formula , detection limit , food science , mathematics , organic chemistry , statistics
In this work, a simple procedure of melamine determination in dairy products is reported. This is based first on melamine extraction from dairy products by 1% acetic acid, sonication, centrifugation and filtration by 0.45 µm filter. The proposed method has a low detection limit (0.50 mg kg −1 ), high accuracy (%recovery 98.9%), high precision (%RSD range 1.6–2.5%), high calibration sensitivity (19,335 (mg l −1 ) −1 ), and a wide dynamic range (1.0–50.0 mg l −1 ). Melamine was accurately quantified in spiked powdered milk, infant powder milk, full‐fat liquid milk, fat‐free liquid milk, local yoghurt, and local soft cheese (spiking levels 0.5, 50, and 1000 mg kg −1 ). The samples have variable amounts of fat (0–29%) and protein (3–23%) indicating the wide applicability of the proposed method. The %recoveries with %RSD were 78.2–103.6(2.5), 92.7–98.8(4.7), 79.3–101.5(3.8), 86.3–101.0(2.6), 78.0–89.2 (8.3), and 91.8–103.8(3.2) for soft cheese, yoghurt, powdered milk, infant powder, full‐fat liquid milk, fat‐free liquid milk, respectively. Practical Applications A simple and accurate analytical method was proposed for quick melamine detection and quantification in milk and dairy products having variable amounts of fat (0–29%) and protein (3–23%) with minimal sample clean up. The method is mainly based on melamine extraction by 1% acetic acid, sonication, centrifugation for 4.0 min, and filtration by 0.45 μm cellulose filter. The method could detect melamine down to 0.50 mg kg −1 with acceptable accuracy and precision (2.5 mg kg −1 is the upper limit of melamine in milk and dairy products). The proposed method was found effective for melamine quantification at three variable spiked levels (0.5, 10, and 1000 mg kg −1 ) in local soft cheese, local yoghurt, powdered milk, infant powder, full‐fat liquid milk, fat‐free liquid milk with %recoveries (%RSD) of 78.2–103.6 (2.5), 92.7–98.8 (4.7), 79.3–101.5 (3.8), 86.3–101.0 (2.6), 78.0–89.2 (8.3), and 91.8–103.8(3.2), respectively.