2018 年 25 巻 2 号 p. 86-91
An analytical method for the determination of histamine in fish meal by LC-MS/MS was developed. Histamine was extracted with 5% trichloroacetic acid. The extract was neutralized and cleaned up with a weak cation ion exchange cartridge (WCX) column. The cartridge was washed with water and methanol, and histamine was eluted with methanol-water (1:1) solution containing 2 % formic acid. Histamine in the eluate was measured by LC-MS / MS. The LC separation was carried out on a Triart Diol-HILIC plus column with a linear gradient of 0.1% formic acid and acetonitrile. MS was carried out in the positive ion electrospray ionization mode. Recovery tests of histamine from seven kinds of fish meal and four kinds of assorted feed were 79.6 to 116%, and the relative standard deviation were 1.9 to 10.3%. The limits of quantitation of the developed method was 5 mg/kg.