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采用快速、简便、廉价、有效、耐用和安全的提取程序以及超高效液相色谱-串联质谱法同时测定有机产品中的农药、生物农药和霉菌毒素。

Simultaneous determination of pesticides, biopesticides and mycotoxins in organic products applying a quick, easy, cheap, effective, rugged and safe extraction procedure and ultra-high performance liquid chromatography-tandem mass spectrometry.

机构信息

Group "Analytical Chemistry of Contaminants", Department of Analytical Chemistry, Almeria University, E-04071 Almeria, Spain.

出版信息

J Chromatogr A. 2011 Mar 18;1218(11):1477-85. doi: 10.1016/j.chroma.2011.01.034. Epub 2011 Jan 19.

Abstract

A method for the simultaneous determination of pesticides, biopesticides and mycotoxins from organic products was developed. Extraction of more than 90 compounds was evaluated and performed by using a modified QuEChERS-based (acronym of Quick, Easy, Cheap, Effective, Rugged, and Safe) sample preparation procedure. The method was based on a single extraction with acidified acetonitrile, followed by partitioning with salts, avoiding any clean-up step prior the determination by ultra-high performance liquid chromatography/tandem quadrupole mass spectrometry (UHPLC-MS/MS). Validation studies were carried out in wheat, cucumber and red wine as representative matrixes. Recoveries of the spiked samples were in the range between 70 and 120% (with intra-day precision, expressed as relative standard deviation, lower than 20%) for most of the analysed compounds, except picloram and quinmerac. Inter-day precision, expressed as relative standard deviation, was lower than 24%. Limits of quantification were lower than 10μg kg⁻¹ and the developed method was successfully applied to the analysis of organic food products, detecting analytes belonging to the three types of compounds.

摘要

建立了一种用于同时测定有机产品中农药、生物农药和霉菌毒素的方法。采用改良的基于 QuEChERS(Quick、Easy、Cheap、Effective、Rugged、and Safe 的缩写)的样品制备程序对 90 多种化合物进行了评估和提取。该方法基于用酸化乙腈进行的单次提取,然后用盐进行分配,避免在通过超高效液相色谱/串联四极杆质谱法(UHPLC-MS/MS)进行测定之前进行任何净化步骤。在小麦、黄瓜和红酒作为代表性基质中进行了验证研究。除了百草枯和苯氧喹外,大多数分析化合物的加标样品回收率在 70%至 120%之间(日内精密度表示为相对标准偏差,低于 20%)。日间精密度表示为相对标准偏差,低于 24%。定量限低于 10μg kg⁻¹,该方法成功应用于有机食品产品的分析,检测到属于这三种类型化合物的分析物。

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