To
develop a rapid detection method for nonprotein nitrogen adulterants,
this experiment sets up a set of point-scan Raman hyperspectral imaging
systems to qualitatively distinguish and quantitatively and positionally
analyze samples spiked with a single nonprotein nitrogen adulterant
and samples spiked with a mixture of nine nonprotein nitrogen adulterants
at different concentrations (5 × 10–3 to 2.000%,
w/w). The results showed that for samples spiked with single nonprotein
nitrogen adulterants, the number of pixels corresponding to the adulterant
in the region of interest increased linearly with an increase in the
analyte concentration, the average coefficient of determination (R
2) was above 0.99, the minimum detection concentration
of nonprotein nitrogen adulterants reached 0.010%, and the relative
standard deviation (RSD) of the predicted concentration was less than
6%. For the sample spiked with a mixture of nine nonprotein nitrogen
adulterants, the standard curve could be used to accurately predict
the additive concentration when the additive concentration was greater
than 1.200%. The detection method established in this study has good
accuracy, high sensitivity, and strong stability. It provides a method
for technical implementation of real-time and rapid detection of adulterants
in milk powder at the port site and has good application and promotion
prospects.
An analytical method has been developed for the detection of a metabolite of nifursol, 3,5-dinitrosalicylic acid hydrazide, in foodstuffs of animal origin (chicken liver, pork liver, lobster, shrimp, eel, sausage, and honey). The method combines liquid chromatography and tandem mass spectrometry with liquid-liquid extraction. Samples were hydrolyzed with hydrochloric acid and derivatized with 2-nitrobenzaldehyde at 37°C for 16 h. The solutions of derivatives were adjusted to pH 7.0-7.5, and the metabolite was extracted with ethyl acetate. 3,5-Dinitrosalicylic acid hydrazide determination was performed in the negative electrospray ionization method. Both isotope-labeled internal standard and matrix-matched calibration solutions were used to correct the matrix effects. Limits of quantification were 0.5 μg/kg for all samples. The average recoveries, measured at three concentration levels (0.5, 2.0, and 10 μg/kg) were in the range of 75.8-108.4% with relative standard deviations below 9.8%. The developed method exhibits a high sensitivity and selectivity for the routine determination and confirmation of the presence of a metabolite of nifursol in foodstuffs of animal origin.
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