The invention relates to the technical field of
analytical chemistry detection, in particular to a method for determining trace
nitrite in pharmaceutic adjuvants. The method comprises the following steps: weighing a
test sample, placing the
test sample in a measuring flask, adding
acetonitrile according to a ratio, and dispersing the sample by vortex oscillation; adding a pre-prepared
nitrite reference
stock solution, adding water, shaking, mixing and diluting, and shaking uniformly to obtain a
standard test solution; preparing a standard-free
test solution which does not contain the reference
stock solution as a reference; taking supernate of the labeled
test sample solution, enabling the supernate to sequentially pass through an activated silver column and an activated
sodium column, filtering the supernate through a PES filter membrane, discarding initial filtrate, and collecting subsequent filtrate for later use; measuring the
nitrite reference substance
stock solution, diluting the nitrite reference substance stock solution with an
acetonitrile-water mixed
solvent, and preparing reference substance solutions with different concentrations for later use; a labeled
test solution, a non-labeled
test solution and reference solutions with different concentrations are respectively subjected to sample introduction detection under preset
ion chromatography conditions, so that the content of trace nitrite in the
pharmaceutic adjuvant can be accurately and quantitatively determined.