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Detecting the total melamine method in food
At present, several analytical techniques are used for detecting melamine, with high-performance liquid chromatography (HPLC), gas chromatography (GC), and liquid chromatography being among the most commonly employed methods. This article compiles some domestic research studies and organizes them to provide a comprehensive overview of current detection approaches. These methods include GC-MS, Spectra-Quad online analysis, ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS), reversed-phase HPLC, HPLC-diode array detection, HPLC-quadrupole mass spectrometry, solid-phase extraction coupled with HPLC, and liquid chromatography-tandem mass spectrometry (LC-MS/MS).
One method involves the use of ultra-performance liquid chromatography with electrospray ionization tandem mass spectrometry for determining residual melamine in feed. The sample was extracted using 1% trichloroacetic acid and dimethyl sulfoxide, purified with an MCX column, and analyzed by UPLC-ESI-MS/MS. The linear range was between 10 and 5,000 μg/kg (r > 0.99), with recovery rates between 83% and 94%, and a detection limit of 10 μg/kg.
Another approach uses HPLC-quadrupole mass spectrometry for melamine detection in feed. With solid-phase extraction and optimized MS conditions, this method demonstrated a linear range of 0.01–0.50 μg/mL, with relative standard deviations below 7.7% and recoveries between 72.4% and 91.2%.
For pet food, LC-MS/MS has been developed as a highly sensitive and selective method. Compared to GC-MS and LC methods from the US FDA, LC-MS/MS offers simpler pretreatment and better performance. Similarly, LC-MS/MS was used to detect melamine in feed samples, showing good linearity and accuracy.
A solid-phase extraction-LC-MS/MS method was also applied to food samples, with a linear range of 0.1–10.0 mg/kg, correlation coefficient r = 0.9999, and detection limit of 0.5 mg/kg.
The Spectra-Quad online analyzer from Thermo Fisher Scientific provides real-time, non-contact detection of melamine using near-infrared absorption technology. This method is unaffected by protein content, making it ideal for continuous monitoring in production lines.
In terms of HPLC methods, reversed-phase HPLC was used for feed analysis, while the diode array method was applied to high-protein foods. Both methods showed excellent precision and sensitivity. Additionally, HPLC with a C18 column and UV detection provided a simple and reliable method for melamine quantification in feed, with a linear range of 1–100 mg/L.
Finally, solid-phase extraction combined with HPLC was successfully used to determine melamine in pet food, demonstrating the versatility and effectiveness of these techniques in various applications.