Detection method of free and combined carboxy methyl lysine in milk and dairy products
A technology of carboxymethyl lysine and a detection method, which is applied in the field of isotope dilution high performance liquid chromatography tandem ion trap mass spectrometry, can solve the problems of increasing retention time, damage to mass spectrometry instruments, narrow use range and the like, so as to improve quantitative accuracy , the effect of increasing the linear range and saving usage
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[0028] In order to better understand the technical solution of the present invention, the technical solution provided by the present invention is described in detail below in conjunction with examples, but the present invention is not limited in any way.
[0029] 1. Sample pretreatment: Accurately weigh 0.1g of solid milk powder sample, add 1mL of ultrapure water and vortex to mix to make a sample solution, directly measure 1mL of liquid dairy products; add 2-3mL of n-hexane to the sample preparation solution , after shaking well, centrifuge at 4000r / min for 10min, discard the n-hexane layer, weigh 2-3 times to completely remove fat, skim milk and milk powder can skip this step; add 1.5mL of 0.2mol / L, pH9.4 Sodium borate buffer solution, 1mL sodium borohydride solution, react at 4°C for 6h; add 60% trichloroacetic acid solution twice the volume of the sample, centrifuge at 8000r / min, 4°C for 10min, separate supernatant and protein precipitate, collect separately and wait for F...
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