Abstract
A method for rapid and sensitive determination of melamine in aquatic products by gas chromatography–mass spectrometry with microwave-assisted derivatization was proposed in this paper. Melamine was extracted from aquatic product samples using methanol, and the extract was cleaned with a mixed-mode cationic exchange solid phase extraction column. After elution with 5 % ammonia–methanol solution and drying with nitrogen, the residue was derivatized using N,O-bis(trimethylsilyl)trifluoroacetamide containing 1 % trimethylchlorosilane under microwave irradiation for 1 min with a power of 420 W, then detected with gas chromatography–mass spectrometry, and quantified by the external standard method. Some important parameters such as extraction solvent, microwave irradiation power and time, and derivatization reagent volume were investigated and optimized. The results showed that methanol could effectively extracted melamine from aquatic products as well as precipitated the protein in samples. Under the optimum conditions, the detection limit for melamine was as low as 0.006 mg/kg, and the linear range was from 0.02 to 50 mg/kg with a correlation coefficient of 0.9997. The proposed method was applied to the analysis of melamine in aquatic products (fish, shrimp, clam, and winkle), and the recovery for melamine was 89.65–105.16 % with relative standard deviation of 3.0–6.0 %.
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The financial support from the National Natural Science Foundation of China (No. 41071315) is greatly appreciated.
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Yanping Zhang declares that she has no conflict of interest. Xiaoguo Ma declares that he has no conflict of interest. Yingming Fan declares that he has no conflict of interest. This article does not contain any studies with human or animal subjects.
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Yanping Zhang and Yingming Fan contributed equally to this work.
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Zhang, Y., Ma, X. & Fan, Y. A Rapid and Sensitive Method for Determination of Melamine in Fish, Shrimp, Clam, and Winkle by Gas Chromatography–Mass Spectrometry with Microwave-Assisted Derivatization. Food Anal. Methods 7, 1763–1769 (2014). https://doi.org/10.1007/s12161-014-9810-1
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DOI: https://doi.org/10.1007/s12161-014-9810-1