Fukumitsu Toru, Waki Masumi, Hagio Masahito, Hayashi Takako, Kuwahara Chikako
Kanagawa Prefectural Institute of Public Health.
Shokuhin Eiseigaku Zasshi. 2021;62(5):168-174. doi: 10.3358/shokueishi.62.168.
In this study, we developed an analytical method for simultaneous determination of 14 quinolones and 4 tetracyclines in livestock and fishery products using LC-MS/MS. The analytes were extracted from food samples with citrate buffer (containing EDTA)-methanol-acetonitrile (3 : 1 : 1, v/v/v) in the presence of n-hexane, and the extract was purified with an Oasis PRiME HLB cartridge column. It was suggested that this analytical method can also extract analytes from solid samples containing fat by using n-hexane. In addition, using methanol-acetonitrile (3 : 7, v/v) containing 0.1 vol% formic acid as an eluent from the cartridge column, the purification effect could be improved, while minimizing the impairment of the recovery rate. As a result of the validation using six types of food samples, trueness (accuracy) was 70.6%-113.8%, the RSD of repeatability was 9.0% or less, and the RSD of within-laboratory reproducibility was 15.5% or less. Using this approach, the standard values mentioned in the Japanese guideline were successfully met.
在本研究中,我们开发了一种使用液相色谱-串联质谱法(LC-MS/MS)同时测定畜禽和水产品中14种喹诺酮类药物和4种四环素类药物的分析方法。在正己烷存在的情况下,用柠檬酸缓冲液(含乙二胺四乙酸)-甲醇-乙腈(3:1:1,v/v/v)从食品样品中提取分析物,提取物用Oasis PRiME HLB柱净化。结果表明,该分析方法也可通过使用正己烷从含脂肪的固体样品中提取分析物。此外,使用含0.1%(体积分数)甲酸的甲醇-乙腈(3:7,v/v)作为柱洗脱液,可提高净化效果,同时将回收率的损失降至最低。通过对六种食品样品的验证,准确度(准确性)为70.6%-113.8%,重复性相对标准偏差(RSD)为9.0%以下,实验室内再现性RSD为15.5%以下。采用该方法成功达到了日本指南中提及的标准值。