LC-MS/MSによるアユ（<i>Plecoglossus altivelis</i>）中のフェニコール系薬剤の分析

Abstract

An analytical method for the determination of residues of 3 phenicol drugs (chloramphenicol, thiamphenicol and florfenicol) in Ayu (Plecoglossus altivelis) by LC-MS/MS was developed. We used the whole body of Ayu, including the bones and internal organs, in addition to muscle. Phenicols were extracted with 90% acetonitrile and an aliquot of the crude extract was cleaned up on a Florisil column (2 g), followed by defatting with n-hexane. The acetonitrile extract was evaporated and the solvent was replaced with phosphate buffer, then the extract was purified on a hydroxylated styrene-divinylbenzene copolymer column (200 mg). Finally, sample solution was passed through a deproteination cartridge filter with a lipid removal function. Chloramphenicol was quantitated by means of a calibration curve corrected with salogate standard (chloramphenicol-d5) and thiamphenicol and florfenicol were quantitated based on absolute calibration curves. This method was validated in accordance with the notification of the Ministry of Health, Labour and Welfare of Japan. As a result of the validation study, the trueness, repeatability and within-laboratory reproducibility were 85-103, 5-13 and 8-13%, respectively. This method is useful for inspecting residues of 3 phenicol drugs in whole body of Ayu efficiently. Moreover, when chloramphenicol and thiamphenicol are detected by this method, the quantitated value is applicable to decide the compliance of the sample with the specifications and standards of the Food Sanitation Law.