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Stable Isotope Dilution Assay for the Accurate Determination of Mycotoxins in Maize by UHPLC-MS/MS

机译:UHPLC-MS / MS稳定同位素稀释法准确测定玉米中的真菌毒素

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A fast,easy-to-handle and cost-effective analytical method for 11 mycotoxins currently regulated in maize and other cereal-based food products in Europe was developed and validated for maize.The method is based on two extraction steps using different acidified acetonitrile-water mixtures.Separation is achieved using ultrahigh-performance liquid chromatography (UHPLC) by a linear water-methanol gradient.After electrospray ionisation,tandem mass spectrometric detection is performed in dynamic multiple reaction monitoring mode.Since accurate mass spectrometric quantification is hampered by matrix effects,uniformly [13 C]-labelled mycotoxins for each of the 11 compounds were added to the sample extracts prior to UHPLC-MS/MS analysis.%欧洲目前针对玉米及其他谷类食物,要求控制11种霉菌毒素的含量,为此开发出了一种便于操作且具有成本效率的分析方法,而且通过玉米得到了验证.此方法基于两个萃取步骤,而这两个步骤采用了不同的经酸化的乙腈-水混合液.分离是通过线性水-甲醇梯度超高效液相色谱法(UHPLC)完成的.在电喷雾电离之后,以动态多反应监测模式进行串联质谱检测.由于基质效应会妨碍精密的质谱定量分析,在进行UHPLC-MS/MS分析前,统一向样品萃取物加入分别与11种化合物相对应的[13C]-标记霉菌毒素.在萃取之前以及之后,以霉菌毒素加入空白玉米样品取得方法性能参数,此试验采用三个平行样,针对6个水平进行.双重萃取后两步萃取总所有目标分析物(包括伏马菌素)回收率在97%到111%之间.
机译:A fast,easy-to-handle and cost-effective analytical method for 11 mycotoxins currently regulated in maize and other cereal-based food products in Europe was developed and validated for maize.The method is based on two extraction steps using different acidified acetonitrile-water mixtures.Separation is achieved using ultrahigh-performance liquid chromatography (UHPLC) by a linear water-methanol gradient.After electrospray ionisation,tandem mass spectrometric detection is performed in dynamic multiple reaction monitoring mode.Since accurate mass spectrometric quantification is hampered by matrix effects,uniformly [13 C]-labelled mycotoxins for each of the 11 compounds were added to the sample extracts prior to UHPLC-MS/MS analysis.%欧洲目前针对玉米及其他谷类食物,要求控制11种霉菌毒素的含量,为此开发出了一种便于操作且具有成本效率的分析方法,而且通过玉米得到了验证.此方法基于两个萃取步骤,而这两个步骤采用了不同的经酸化的乙腈-水混合液.分离是通过线性水-甲醇梯度超高效液相色谱法(UHPLC)完成的.在电喷雾电离之后,以动态多反应监测模式进行串联质谱检测.由于基质效应会妨碍精密的质谱定量分析,在进行UHPLC-MS/MS分析前,统一向样品萃取物加入分别与11种化合物相对应的[13C]-标记霉菌毒素.在萃取之前以及之后,以霉菌毒素加入空白玉米样品取得方法性能参数,此试验采用三个平行样,针对6个水平进行.双重萃取后两步萃取总所有目标分析物(包括伏马菌素)回收率在97%到111%之间.

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