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1.
Analyst ; 142(10): 1682-1688, 2017 May 15.
Article in English | MEDLINE | ID: mdl-28181598

ABSTRACT

The implausible combination of centrifugal disc microfluidics and un-covered channels provides a simple way in which Raman spectroscopy can be implemented in industrially-relevant lab-on-a disc technology. Here we demonstrate these advantages by detecting very low concentrations of melamine in liquid milk, without pre-processing, without surface enhancement of the Raman signal and with no evidence of spectral contamination from the polymeric chip itself. A limit of detection (LOD) of 203 ppm for melamine in milk was achieved from Raman spectra of milk after drying. The centrifugal disc rotation and microchannel geometry results in rapid and reliable filling of the channels and in meniscus shape control, enabling reproducible Raman detection with quantitative precision.

2.
J Dairy Sci ; 99(10): 7821-7831, 2016 Oct.
Article in English | MEDLINE | ID: mdl-27474982

ABSTRACT

We have developed a powerful general spectroscopic method for rapidly screening liquid milk for adulterants by combining reflective focusing wells simply fabricated in aluminum with a small, portable Raman spectrometer with a focusing fiber optic probe. Hemispherical aluminum sample wells were specially designed to optimize internal reflection and sampling volume by matching the focal length of the mirror to the depth of focus of the laser probe. The technique was tested on milk adulterated with 4 different nitrogen-rich compounds (melamine, urea, dicyandiamide, and ammonium sulfate) and sucrose. No sample preparation of the milk was needed, and the total analysis time was 4min. Reliable sample presentation enabled average reproducibility of 8% residual standard deviation. The limit of detection interval measured from partial least squares calibrations ranged between 140 and 520mg/L for the 4 N-rich compounds and between 7,000 and 36,000mg/L (0.7-3.6%) for sucrose. The portability of the system and the reliability and reproducibility of this technique open opportunities for general, reagentless screening of milk for adulterants at the point of collection.


Subject(s)
Food Contamination , Milk/chemistry , Animals , Calibration , Nitrogen Compounds , Reproducibility of Results , Triazines
3.
J Dairy Sci ; 99(4): 2520-2536, 2016 Apr.
Article in English | MEDLINE | ID: mdl-26874427

ABSTRACT

Adulteration of milk for commercial gain is acknowledged as a serious issue facing the dairy industry. Several analytical techniques can be used to detect adulteration but they often require time-consuming sample preparation, expensive laboratory equipment, and highly skilled personnel. Here we show that Raman spectroscopy provides a simple, selective, and sensitive method for screening milk, specifically for small nitrogen-rich compounds, such as melamine, urea, ammonium sulfate, dicyandiamide, and for sucrose. Univariate and multivariate statistical methods were used to determine limits of detection and quantification from Raman spectra of milk spiked with 50 to 1,000 mg/L of the N-rich compounds and 0.25 to 4% sucrose. Partial least squares (PLS) calibration provided limit of detection minimum thresholds <200mg/L (0.02%) for the 4 N-rich compounds and <0.8% for sucrose, without the need for surface-enhanced Raman spectroscopy. The results show high reproducibility (7% residual standard deviation) and 100% efficiency for screening of milk for these adulterants.


Subject(s)
Milk/chemistry , Spectrum Analysis, Raman/methods , Animals , Calibration , Nitrogen/analysis , Nitrogen Compounds/analysis , Reproducibility of Results , Sucrose/analysis , Triazines/analysis
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