The invention relates to the technical field of medical detection, and specifically relates to a method for measuring the concentration of
phenylephrine in
plasma by LC-MS / MS. The method comprises thefollowing steps: primary extraction: adding an
internal standard working solution and an extracting solution into a sample, centrifugally layering the solution after mixing the solutions uniformly, and collecting the supernatant to obtain first supernatant;
derivatization reaction: concentrating and
drying the first supernatant, adding a NaHCO3 buffer salt for
dissolution, and then adding an
acetonitrile solution of
dansyl chloride to perform a
derivatization reaction; and secondary extraction: adding the extracting solution into the reaction solution after the
derivatization reaction for secondary extraction, centrifuging to obtain second supernatant, concentrating and
drying the second supernatant, and redissolving the product to obtain a sample solution. By adoption of the
pretreatment method of the sample provided by the invention, the extraction rate of low-level
phenylephrine can be maximally improved, the interference of a
plasma matrix is effectively removed, the specificityis improved, the minimum
detection limit is reduced to 0.02ng / ml, and the sensitivity is increased to 0.1nM to adapt to the detection requirements of the concentration of the low-concentration
phenylephrine in
drug clinical studies.