Ishii R, Horie M, Chan W, MacNeil J
Department of Water and Food, Saitama Prefectural Institute of Public Health, Saitama, Japan.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2008 Dec;25(12):1509-19. doi: 10.1080/02652030802189740.
Quantitative methods using liquid chromatography coupled with tandem mass spectrometry were developed for seven kinds of aminoglycoside antibiotics in kidney and muscle tissues. Mass spectral acquisition was performed in the positive-ion mode by applying multiple reaction monitoring. Liquid chromatographic separation employed a ZIC-HILIC column (SeQuant) for hydrophilic interaction chromatography. Extraction of the aminoglycosides was performed using liquid extraction with a phosphate buffer containing trichloroacetic acid, followed by a solid-phase clean-up procedure on a weak cation-exchange column with carboxypropyl (CBX) SPE cartridge (Mallinckrodt Baker). The limits of quantification were 25 ng g(-1) for gentamicin, 50 ng g(-1) for spectinomycin, dihydrostreptomycin, kanamycin and apramycin, and 100 ng g(-1) for streptomycin and neomycin. These are well below the maximum residue limits set by the Codex Alimentarius Commission. The recoveries of all compounds from all tissues fortified at the level of quantification limits of 500 and 1000 ng g(-1) were >70%, and the variability (relative standard deviation) was generally <12%.
建立了采用液相色谱-串联质谱联用的定量方法,用于检测肾脏和肌肉组织中的七种氨基糖苷类抗生素。通过多反应监测在正离子模式下进行质谱采集。液相色谱分离采用ZIC-HILIC柱(SeQuant)进行亲水相互作用色谱分析。氨基糖苷类的提取采用含三氯乙酸的磷酸盐缓冲液进行液液萃取,随后在含羧丙基(CBX)的弱阳离子交换柱固相萃取柱(Mallinckrodt Baker)上进行净化。庆大霉素的定量限为25 ng g(-1),壮观霉素、二氢链霉素、卡那霉素和安普霉素的定量限为50 ng g(-1),链霉素和新霉素的定量限为100 ng g(-1)。这些均远低于食品法典委员会设定的最大残留限量。在500和1000 ng g(-1)定量限水平下对所有组织中所有化合物的回收率均>70%,且变异性(相对标准偏差)通常<12%。