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一种用于定量分析牛基质中百里香酚和香芹酚并测定牛奶和组织中残留消除情况的顶空固相微萃取-气相色谱-串联质谱法的开发。

Development of a HS-SPME-GC-MS/MS Method for the Quantitation of Thymol and Carvacrol in Bovine Matrices and To Determine Residue Depletion in Milk and Tissues.

作者信息

Armorini Sara, Yeatts James E, Mullen Keena A E, Mason Sharon E, Mehmeti Elmira, Anderson Kevin L, Washburn Steve P, Baynes Ronald E

机构信息

Department of Veterinary Medical Sciences, University of Bologna , 40064 Ozzano dell'Emilia, Bologna, Italy.

Department of Biological Sciences, Campbell University , Buies Creek, North Carolina 27506, United States.

出版信息

J Agric Food Chem. 2016 Oct 19;64(41):7856-7865. doi: 10.1021/acs.jafc.6b02899. Epub 2016 Oct 11.

Abstract

Thymol and carvacrol may be present in several phytoceutical products but there are no well-defined methods to measure these compounds in meat and milk from treated animals. U.S. regulatory authorities deem their presence as an adulteration of food. A rapid and sensitive HS-SPME-GC-MS/MS method was developed for the detection of thymol and carvacrol in bovine milk, plasma, liver, kidney, and fat. Inter- and intraday precision values were all less than 15.7 and 20.2% for thymol and carvacrol, respectively. The accuracy was in ranges of 69.9-111.8% for thymol and 74.0-119.2% for carvacrol. With the exception of fat tissue, stability studies showed that both compounds are stable over a 2 month period. A pilot pharmacokinetic study was conducted to evaluate the developed analytical method and to provide initial estimates of thymol and carvacrol depletion in plasma, milk, and several tissues. Treatment of lactating dairy cattle with phytoceutical products containing these substances resulted in low but measurable residue levels at 96 h for liver and 36 h for milk with very short apparent plasma and milk half-lives (<3.0 h).

摘要

百里香酚和香芹酚可能存在于多种植物药产品中,但目前尚无明确的方法来测定经处理动物的肉和奶中的这些化合物。美国监管当局认为它们的存在属于食品掺假行为。本文建立了一种快速灵敏的顶空固相微萃取-气相色谱-串联质谱法(HS-SPME-GC-MS/MS),用于检测牛乳、血浆、肝脏、肾脏和脂肪中的百里香酚和香芹酚。百里香酚和香芹酚的日间和日内精密度值分别均小于15.7%和20.2%。百里香酚的准确度在69.9%-111.8%之间,香芹酚的准确度在74.0%-119.2%之间。稳定性研究表明,除脂肪组织外,这两种化合物在2个月内均保持稳定。开展了一项初步药代动力学研究,以评估所建立的分析方法,并初步估计血浆、乳汁和几种组织中百里香酚和香芹酚的消除情况。用含有这些物质的植物药产品对泌乳奶牛进行处理后,肝脏在96小时时、乳汁在36小时时会残留低但可测量的水平,其血浆和乳汁的表观半衰期非常短(<3.0小时)。

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