{"title":"[Determination of Chlorothalonil Metabolite I in Livestock Products by LC-MS/MS].","authors":"Maki Kobayashi, Naoko Sakai, Yuki Ohmachi, Yuka Morita, Satoru Nemoto, Kenji Ohtsuka","doi":"10.3358/shokueishi.63.195","DOIUrl":null,"url":null,"abstract":"<p><p>An analytical method based on LC-MS/MS was developed for the determination of chlorothalonil metabolite I in livestock products. Chlorothalonil metabolite I 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 silica gel (SI) 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 chlorothalonil metabolite I from five types of livestock products (cattle muscle, cattle fat, cattle liver, milk and egg) spike at the maximum residue limits (MRLs) or at a uniform limit of 0.01 mg/kg was 97.1-102.9%, with a relative standard deviation of 1.4-6.8%. The limit of quantitation of the developed method was calculated to be 0.01 mg/kg.</p>","PeriodicalId":54373,"journal":{"name":"Food Hygiene and Safety Science","volume":"63 6","pages":"195-201"},"PeriodicalIF":0.2000,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Food Hygiene and Safety Science","FirstCategoryId":"97","ListUrlMain":"https://doi.org/10.3358/shokueishi.63.195","RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"FOOD SCIENCE & TECHNOLOGY","Score":null,"Total":0}
引用次数: 0
Abstract
An analytical method based on LC-MS/MS was developed for the determination of chlorothalonil metabolite I in livestock products. Chlorothalonil metabolite I 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 silica gel (SI) 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 chlorothalonil metabolite I from five types of livestock products (cattle muscle, cattle fat, cattle liver, milk and egg) spike at the maximum residue limits (MRLs) or at a uniform limit of 0.01 mg/kg was 97.1-102.9%, with a relative standard deviation of 1.4-6.8%. The limit of quantitation of the developed method was calculated to be 0.01 mg/kg.
建立了畜产品中百菌清代谢物I的LC-MS/MS分析方法。用丙酮提取畜产品中的百菌清代谢物I。采用乙腈和正己烷分馏法对粗提物进行脱脂。在酸性条件下，使用乙二胺- n -丙基硅基化硅胶(PSA)和硅胶(SI)微型柱的组合进行清理。采用外溶剂校准曲线对样品溶液进行LC-MS/MS分析。5种畜产品(牛肌肉、牛脂肪、牛肝脏、牛奶和鸡蛋)中百菌清代谢产物I在最大残留限量(MRLs)和统一限量为0.01 mg/kg时的平均回收率(n=5)为97.1-102.9%，相对标准偏差为1.4-6.8%。方法的定量限为0.01 mg/kg。
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