Determination of melamine in milk powder using zwitterionic HILIC stationary phase with UV detection

Abstract

A hydrophilic interaction liquid chromatography-UV method was developed for the determination of melamine in milk powder. Sulfobetaine type zwitterionic hydrophilic interaction liquid chromatography stationary phase was used to achieve straightforward separation of melamine in milk powder without any sample derivatization or addition of ion-pair reagent. The sample preparation was simple and fast with the steps of acetonitrile/perchloric acid extraction-centrifugation-filtration. No SPE or other pre-concentration procedure was required. By using large volume sample injection and choosing low UV wavelength (210 nm), the LOD and LOQ were 0.005 and 0.015 microg/mL for melamine standards, and 0.02 and 0.06 microg/mL for the spiked milk extracts. The LOD and LOQ of the latter correspond to 0.95 and 2.2 microg/g melamine in the milk powder. The correlation coefficients for melamine standard, pre-spiked milk extracts and post-spiked milk extracts in the range of 0-0.5 microg/mL were 0.9978, 0.9976 and 0.9995, respectively. This newly developed method is sensitive and cost effective, therefore, suitable for screening of melamine in tainted milk products.

Visual detection of melamine in raw milk by label-free silver nanoparticles

“…The maximum residue level of melamine in infant formula is legally regulated at 1 ppm by Chinese government after the melamine accident (Guo et al, 2010). Currently, several methods have been employed for the determination of melamine in milk and milkbased products, such as gas chromatography (GC) (Yokley, Mayer, Rezaaiyan, Manuli, & Cheung, 2000), high performance liquid chromatography (HPLC) (Ihunegbo, Tesfalidet, & Jiang, 2010;Sun, Wang, Ai, Liang, & Wu, 2010, Venkatasami & Sowa, 2010, high performance liquid chromatography/mass spectrum (HPLC/MS) (Heller & Nochetto, 2008& Kim et al, 2008, surface enhanced Raman spectroscopy (Lin, He, Awika, Yang, Ledoux, & Mustapha, 2008), capillary zone electrophoresis mass spectrum (CE/MS) (Cook, Klampfl, & Buchberger, 2005), and immunoassay analysis (ELISA) (Garber, 2008). These methods have high sensitivity, but most of them are time-consuming and labor-intensive due to the complicated pretreatment of sample, and require expensive instrumentation and high personnel cost.…”

Simultaneous determination of melamine and related compounds by hydrophilic interaction liquid chromatography–electrospray mass spectrometry

“…Various techniques including HPLC-UV [10][11][12] or hydrophilic interaction liquid chromatography (HILIC)-UV [13], HPLC-MS [14][15][16][17][18][19][20][21][22][23][24], GC-MS [24][25][26], desorption ionization MS [27], CE [28][29][30], electrochemical method [31], etc., have been used to detect melamine or cyanuric acid. For the simultaneous determination of melamine and cyanuric acid, HPLC-MS [32] and MALDI-MS [33] were employed.…”

Rapid and High-Throughput Determination of Melamine in Milk Products and Eggs by Full Automatic On-line Polymer Monolith Microextraction Coupled to High-Performance Liquid Chromatography

“…2009; Zhou et al 2009a;Nkem Ihunegbo et al 2010;Desmarchelier et al 2009;Heller and Nochetto 2008;Kim et al 2010), gas chromatography ), thin-layer chromatography (Broszat et al 2008), ultra-performance liquid chromatography (Xia et al 2009) and some others, have been developed to monitor MEL in milk products, eggs as well as other foods and components.…”