4.7 Article

Using activated attapulgite as sorbent for solid-phase extraction of melamine in milk formula samples

Journal

ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 408, Issue 24, Pages 6671-6677

Publisher

SPRINGER HEIDELBERG
DOI: 10.1007/s00216-016-9779-2

Keywords

Attapulgite; Hydrophilic interaction; Ion exchange interaction; Milk formula sample; Solid-phase extraction

Funding

  1. National Natural Science Foundation of China [21405085]
  2. Public Applied Research Programs of Technology of Zhejiang Province [2015C37015]
  3. Zhejiang Provincial Natural Science Foundation of China [LQ12B05001]
  4. Ningbo Natural Science Foundation of China [2012A610091]

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In this study, a simple solid-phase extraction (SPE) approach by using activated attapulgite as sorbent was successfully developed for the determination of melamine in milk formula samples. Crucial factors impacting the extraction efficiency, including sample solvent, elution solvent, and sample loading volume, were investigated. Under the optimal extraction conditions, the sample loading volume was up to 200 mL and the adsorption capacity of the melamine gave rise to 1154 mu g g(-1). Excellent linear calibration curves (r (2) > 0.999) were achieved, and then the limit of detection (S/N = 3) and the limit of quantification (S/N = 10) were found to be 0.15 and 0.5 ng mL(-1), respectively. The recoveries of the melamine spiked in four milk formula samples at three concentration levels ranged from 83.5 to 111.0 % with relative standard deviations (RSDs) less than 10.2 %. Furthermore, RSDs of batch to batch (n = 4) of the acidified attapulgite used in this developed method were in the range of 2.3 similar to 7.3 %. In comparison to the commercial Oasis MCX, the acidified attapulgite sorbent even outperformed (at least in terms of reproducibility) for melamine analysis in real food samples. Because of its simplicity, the newly developed SPE method based on acidified attapulgite nanoparticles should provide a promising tool for daily monitoring of doped melamine in milk formula or other complex matrices.

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