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Molecular species fingerprinting and quantitative analysis of saffron (Crocus sativus L.) for quality control by MALDI mass spectrometry

机译:藏红花(Crocus sativus L.)的分子种类指纹图谱和定量分析,用于通过MALDI质谱进行质量控制

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Herein we describe a rapid, simple, and reliable method for the quantitative analysis and molecular species fingerprinting of saffron ( Crocus sativus L.) by direct MS and MS/MS analysis. Experimentally, powdered saffron was subjected to a brief treatment with a 0.3% TFA water/acetonitrile solution, and the resulting mixture was directly placed on the MALDI plate for analysis. This approach allowed the detection of the commonly observed crocins C-1–C-6 and flavonols, together with the identification of the unknown highly glycosylated crocins C-7 , C-8 and C-9 , and carotenoid-derived metabolites. The strategy endorsed the simultaneous detection and characterization of saffron and adulterant markers using crude extracts of the adulterant itself and synthetic sets of adulterated authentic saffron samples. The implementation of the strategy was to measure the amount of an unknown adulterant from the crude extract using curcumin as a non-isotopic isobaric internal standard. The relationship between the saffron and curcumin molar ratios were established with a correlation coefficient of 0.9942. The ANOVA regression model was significant, F (1, 72) = 13?595.82, p < 0.001, y = (0.0116 ± 0.0001) x + (?0.1214 ± 0.0086). No matrix effects were observed and good results were obtained with respect to instrumental repeatability (*RSD% < 2%) and LOD (1.1%). The analysis of commercial samples of saffron using the proposed approach showed the suitability of the method for routine analysis (minimal sample preparation and very short measuring time per sample).
机译:本文中,我们描述了一种通过直接MS和MS / MS分析对藏红花(Crocus sativus L.)进行定量分析和分子物种指纹分析的快速,简单和可靠的方法。实验上,将粉红色的藏红花用0.3%TFA水/乙腈溶液进行简短处理,然后将所得混合物直接置于MALDI板上进行分析。这种方法可以检测出常见的番红花C-1–C-6和黄酮醇,并鉴定出未知的高度糖基化的番红花C-7,C-8和C-9以及类胡萝卜素衍生的代谢物。该策略支持使用掺假品本身的粗提物和掺假正宗藏红花样品的合成组同时检测和表征藏红花和掺假标记。该策略的实施是使用姜黄素作为非同位素等压内标来测量粗提物中未知杂质的含量。建立了藏红花和姜黄素摩尔比之间的关系,相关系数为0.9942。方差分析回归模型显着,F(1,72)= 13?595.82,p <0.001,y =(0.0116±0.0001)x +(?0.1214±0.0086)。在仪器重复性(* RSD%<2%)和LOD(1.1%)方面,未观察到基质效应,并获得了良好的结果。使用所提出的方法对番红花的商业样品进行分析表明,该方法适用于常规分析(样品制备最少,每个样品的测量时间很短)。

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