Kobayashi Maki, Sakai Naoko, Ohmachi Yuki, Morita Yuka, Nemoto Satoru, Otsuka Kenji
Tokyo Metropolitan Institute of Public Health.
National Institute of Health Sciences.
Shokuhin Eiseigaku Zasshi. 2021;62(1):1-7. doi: 10.3358/shokueishi.62.1.
An analytical method based on LC-MS/MS was developed for the determination of asulam in livestock products. Asulam in livestock products was extracted with acetone. The crude extracts were defatted by acetonitrile and n-hexane partitioning. Cleanup was carried out using a combination of ethylene diamine-N-propyl silylation silica gel (PSA) and octadecyl silylated silica gel (C) mini columns with acidic condition. The sample solution was subjected to LC-MS/MS using an external solvent calibration curve. The average recovery (n=5) of Asulam from four types of livestock products (bovine muscle, bovine fat, bovine liver and milk) spike at the maximum residue limits (MRLs) or at a uniform limit of 0.01 mg/kg was 92.7-98.7%, with a relative standard deviation of 3.1-11.6%. The limit of quantitation of the developed method was calculated to be 0.01 mg/kg.
建立了一种基于液相色谱-串联质谱法（LC-MS/MS）测定畜产品中莠灭净的分析方法。畜产品中的莠灭净用丙酮提取。粗提物通过乙腈和正己烷分配进行脱脂。在酸性条件下，使用乙二胺-N-丙基硅烷化硅胶（PSA）和十八烷基硅烷化硅胶（C）微型柱组合进行净化。样品溶液采用外标溶剂校准曲线进行LC-MS/MS分析。在最大残留限量（MRLs）或统一限量0.01 mg/kg水平下，对四种畜产品（牛肌肉、牛脂肪、牛肝和牛奶）进行加标回收试验（n = 5），莠灭净的平均回收率为92.7%-98.7%，相对标准偏差为3.1%-11.6%。所建立方法的定量限计算为0.01 mg/kg。
