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Artifact-controlled quantification of folpet and phthalimide in food by liquid chromatography-high resolution mass spectrometry
Food Control ( IF 6 ) Pub Date : 2018-04-09
Flavia Badoud, Marion Ernest, Yves-Alexis Hammel, José Fernando Huertas-Pérez

The European residue definition for the pesticide folpet has changed in 2016 to include its degradation product phthalimide. According to recent studies, phthalimide could also arise from other sources than folpet, including formation in the injector of gas chromatograph systems from the precursor phthalic acid or phthalic anhydride. A liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry (MS) method was developed for the quantification of folpet and phthalimide. High resolution MS was deemed necessary to increase the selectivity via accurate mass, as phthalimide and folpet yielded poor fragmentation. Sample preparation by QuEChERS was optimized to ensure the stability of folpet and to prevent the contamination of phthalimide from external sources. The method was validated on four matrices from four commodity groups (i.e., high water content, high water and acid content, high starch content and dairy products). Linearity was assessed with r2 > 0.99 over the range 5–200 μg kg−1, repeatability ranged between 6.8% and 14.5%, intermediate precision between 10% and 23.8%, and trueness was within 78.6% and 124.2% with relative standard deviation from 3% to 20%. These performance parameters were all compliant with the analytical requirements stipulated in the SANTE/11813/2017 document. The method was verified on 12 additional matrices from the 4 commodity groups. The present method was suitable for the quantification of folpet and phthalimide in foods while controlling analytical artifact.



中文翻译:

液相色谱-高分辨率质谱法对食品中福尔贝和邻苯二甲酰亚胺的伪像控制定量

欧洲农药残留的残留定义在2016年发生了变化,包括其降解产物邻苯二甲酰亚胺。根据最近的研究,邻苯二甲酰亚胺也可能是从棉囊中以外的其他来源产生的,包括由前体邻苯二甲酸或邻苯二甲酸酐在气相色谱系统的进样器中形成的。开发了一种液相色谱-大气压化学电离质谱(MS)方法,用于定量分析福尔贝特和邻苯二甲酰亚胺。高分辨率MS被认为是通过精确质量提高选择性所必需的,因为邻苯二甲酰亚胺和Folpet产生的碎片很差。QuEChERS进行的样品制备经过优化,可确保棉絮的稳定性并防止邻苯二甲酰亚胺受到外部污染。该方法在来自四个商品组(即高水含量,高水和酸含量,高淀粉含量和乳制品)的四个矩阵上得到了验证。线性度用r评估 在5–200μgkg -1范围内2 > 0.99 ,重复性在6.8%至14.5%之间,中间精度在10%至23.8%之间,真实度在78.6%和124.2%之内,相对标准偏差从3%至20 %。这些性能参数均符合SANTE / 11813/2017文件中规定的分析要求。该方法在4个商品组的12个其他矩阵上得到了验证。本方法适用于在控制分析伪影的同时对食品中的甜菜碱和邻苯二甲酰亚胺进行定量。

更新日期:2018-04-10
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