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首页> 外文期刊>Journal of Agricultural and Food Chemistry >Development of a Stable Isotope Dilution LC-MS/MS Method for the Alternaria Toxins Tentoxin, Dihydrotentoxin, and Isotentoxin
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Development of a Stable Isotope Dilution LC-MS/MS Method for the Alternaria Toxins Tentoxin, Dihydrotentoxin, and Isotentoxin

机译：稳定的同位素稀释液质联用LC-MS / MS方法的开发，用于链格孢菌毒素，毒素，二氢维托辛和异胃托辛

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摘要

For the Alternaria toxins tentoxin, dihydrotentoxin, and isotentoxin, a stable isotope dilution LC—MS/MS method was first developed. Triply deuterated internal standards were prepared via total synthesis and introducing the labels in the last step before cyclization. Method validation was carried out by using potato starch, tomato puree, and white pepper powder as blank matrices. For the three toxins the limits of detection ranged from 0.10 to 0.99 μg/kg. The inter-/intraday relative standard deviations of the method were below 8.8%, and the recoveries ranged between 98 and 115%. Although cyclic peptides are known to show only negligible fragmentation, a low limit of detection was achieved with the optimization of mass spectrometry parameters and cleanup on Cl8-phenyl SPE columns providing a more selective binding of these phenyl-containing cyclic peptides. The method was applied to 103 food samples including bread, cereals, chips, juice, nuts, oil, sauce, seeds, and spices. Of these, 85% were contaminated with tentoxin and 55% were contaminated with dihydrotentoxin, whereas isotentoxin was not quantifiable. Maximal concentrations of tentoxin and dihydrotentoxin were 52.4 and 36.3 μg/kg, respectively, and were both detected in paprika powder.
机译：对于链格孢菌毒素，腱毒素，二氢维托辛和异维托辛，首先开发了一种稳定的同位素稀释LC-MS / MS方法。通过全合成并在环化之前的最后一步引入标记，制备了三重氘代内标。方法验证是通过使用马铃薯淀粉，番茄泥和白胡椒粉作为空白基质进行的。对于这三种毒素，检出限为0.10至0.99μg/ kg。该方法的日间/日间相对标准偏差在8.8％以下，回收率在98％至115％之间。尽管已知环肽仅显示可忽略的片段，但通过优化质谱参数和在Cl8-苯基SPE色谱柱上进行纯化可实现较低的检测限，从而更选择性地结合这些含苯基的环肽。该方法适用于103个食品样品，包括面包，谷物，薯片，果汁，坚果，油，酱料，种子和香料。其中，85％被腱毒素污染，55％被二氢氧还蛋白污染，而异氧还蛋白则无法量化。 Tentoxin和Dihydrotentoxin的最大浓度分别为52.4和36.3μg/ kg，在辣椒粉中均检出。

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