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[一种同时测定畜禽及水产品中喹诺酮类和四环素类药物的分析方法的建立]

[Development of an Analytical Method for Simultaneous Determinationof Quinolones and Tetracyclines in Livestock and Fishery Products].

作者信息

Fukumitsu Toru, Waki Masumi, Hagio Masahito, Hayashi Takako, Kuwahara Chikako

机构信息

Kanagawa Prefectural Institute of Public Health.

出版信息

Shokuhin Eiseigaku Zasshi. 2021;62(5):168-174. doi: 10.3358/shokueishi.62.168.

Abstract

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.

摘要

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。

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