一种利用超高效液相色谱串联质谱技术检测番茄和番茄产品中链格孢菌毒素交链孢、链格孢酚甲基醚和链格孢毒素的方法及其验证

Development and Validation of a LC-ESI-MS/MS Method for the Determination of Alternaria Toxins Alternariol, Alternariol Methyl-Ether and Tentoxin in Tomato and Tomato-Based Products

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中文摘要:本文基于超高效液相色谱串联质谱法开发了一种同时测定番茄和番茄产品中链格孢菌毒素交链孢、链格孢酚甲基醚和链格孢毒素的方法。采用分散液-液微萃取(DLLME)和LC-ESI-MS/MS联用进行霉菌毒素分析,在正离子模式中采用具有ESI接口的液相色谱-液相色谱-质谱联用系统进行串联质谱参数优化,采用DLLME技术以乙腈作分散剂将样本中的霉菌毒素提取到氯仿(100μL)中,以番茄汁作为空白基质进行方法验证,结果显示,检测限和定量限分别为0.7-3.5 ng/g,在25和50 ng/g加标水平下回收率在80%以上,重复性相对标准偏差(RSDR)小于等于0.09,中间重现性(RSDR)小于等于0.15。30个分析样本中有5个检测到一种及以上链格孢毒素,其中交链孢毒素是最常见的链格孢毒素,且含量接近定量限均值3.75 ng/g。
外文摘要:Alternaria species are capable of producing several secondary toxic metabolites in infected plants and in agricultural commodities, which play important roles in food safety. Alternaria alternata turn out to be the most frequent fungal species invading tomatoes. Alternariol (AOH), alternariol monomethyl ether (AME), and tentoxin (TEN) are some of the main Alternaria mycotoxins that can be found as contaminants in food. In this work, an analytical method based on liquid chromatography (LC) tandem mass spectrometry (MS/MS) detection for the simultaneous quantification of AOH, AME, and TEN in tomato and tomato-based products was developed. Mycotoxin analysis was performed by dispersive liquid-liquid microextraction (DLLME) combined with LC-ESI-MS/MS. Careful optimization of the MS/MS parameters was performed with an LC/MS system with the ESI interface in the positive ion mode. Mycotoxins were efficiently extracted from sample extract into a droplet of chloroform (100 mu L) by DLLME technique using acetonitrile as a disperser solvent. Method validation following the Commission Decision No. 2002/657/EC was carried out by using tomato juice as a blank matrix. Limits of detection and quantitation were, respectively, in the range 0.7 and 3.5 ng/g. Recovery rates were above 80%. Relative standard deviations of repeatability (RSDr) and intermediate reproducibility (RSDR) were <= 9% and <= 15%, respectively, at levels of 25 and 50 ng/g. Five out of 30 analyzed samples resulted positive to at least one Alternaria toxin investigated. AOH was the most common Alternaria toxin found, but at levels close to LOQ (average content: 3.75 ng/g).
 
外文关键词:Alternaria, LC-MS/MS, dispersive liquid-liquid microextraction, tomato
作者:Rodriguez-Carrasco, Yelko; Manes, Jordi; Berrada, Houda; Juan, Cristina
作者单位:Univ Valencia, Fac Pharm, Dept Food Chem & Toxicol, Ave Vicent Andres Estelles S-N, E-46100 Burjassot, Spain.
期刊名称:TOXINS
期刊影响因子:3.571
出版年份:2016
出版刊次:11
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  1. 编译服务:农产品质量安全
  2. 编译者:贵淑婷
  3. 编译时间:2017-01-17