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[采用液相色谱-串联质谱法测定畜产品中的氟苯达唑及其代谢物]

[Determination of Flubendazole and Metabolite in Livestock Products Using LC-MS/MS].

作者信息

Okabe Ryo, Nemoto Satoru, Aoyagi Mitsutoshi

机构信息

Hokkaido Institute of Public Health.

National Institute of Health Sciences.

出版信息

Shokuhin Eiseigaku Zasshi. 2023;64(4):130-135. doi: 10.3358/shokueishi.64.130.

Abstract

This study proposes a method to determine flubendazole and metabolite R35475 in livestock products using tandem mass spectrometry coupled with positive ion electrospray ionization. Acetone is used to extract flubendazole and metabolite R35475 from the livestock samples. These extracts were purified using an SCX cartridge column (500 mg). Furthermore, high-performance liquid chromatography was performed on an Inertsil ODS-4 column with a gradient formed using methanol and water, both of which contain 5 mmol/L of ammonium acetate. The recovery tests using bovine muscle, fat, liver, milk, and egg fortified at the maximum residue limits of analytes or 0.005 mg/kg revealed that the trueness (n=5) of flubendazole and metabolite R35475 ranged from 89.4 to 106.4% with a repeatability rate of 1.7-7.8%.

摘要

本研究提出了一种使用串联质谱结合正离子电喷雾电离法测定畜产品中氟苯达唑及其代谢物R35475的方法。用丙酮从畜产品样品中提取氟苯达唑及其代谢物R35475。这些提取物用SCX柱(500毫克)进行纯化。此外,在Inertsil ODS-4柱上进行高效液相色谱分析,使用甲醇和水形成梯度,二者均含有5毫摩尔/升的醋酸铵。在分析物的最大残留限量或0.005毫克/千克水平下对牛肌肉、脂肪、肝脏、牛奶和鸡蛋进行加标回收试验,结果表明,氟苯达唑及其代谢物R35475的真实度(n = 5)在89.4%至106.4%之间,重复性率为1.7%至7.8%。

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