利用 GC/LC-Q-TOF/MS 同时测定当归中的农药、霉菌毒素和阿魏酸

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A Pub Date : 2024-10-12 DOI:10.1016/j.chroma.2024.465437

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引用次数: 0

摘要

本研究建立了一种可同时测定当归中33种农药（54个化合物）、11种真菌毒素和功能成分（阿魏酸）的适用性强的方法。通过优化萃取溶剂的酸度、冰浴和振荡的顺序、体积溶液等条件，提高了样品前处理方法对农药、真菌毒素和功能成分的兼容性。在对四种前处理方法进行比较后，PRiME HLB SPE 前处理方法被选为最佳方法。在 65 种污染物中，有 38 种采用液相色谱法测定，41 种采用气相色谱法测定，其线性关系良好（R2 > 0.9801），97%的污染物的定量限（LOQ）低于 0.02 mg kg-1。在 LOQ、2 倍 LOQ 和 10 倍 LOQ 加标水平下，所有化合物的回收率均在 70% 至 120% 之间，RSD 均低于 20%。阿魏酸的最低检出限为 50 ng/mL，在 0.5 至 10 μg/mL 范围内线性关系良好（R2=0.9988）。回收率和 RSD 分别为 98.1 % 和 3.2 %（n = 6）。通过将 SPE 和 GC/LC-Q-TOF/MS 结合使用，可在单一样品制备过程中同时测定跨类别化合物。因此，该研究不仅缩短了数据采集和数据分析的时间，还提高了实验效率。

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Simultaneous determination of pesticides, mycotoxins and ferulic acid in Angelica sinensis by GC/LC-Q-TOF/MS

In this study, a strong applicable method that could determine a total of 33 pesticides (54 compounds), 11 mycotoxins and functional components (ferulic acid) simultaneously in Angelica sinensis was developed. The compatibility of the sample pretreatment method for pesticides, mycotoxins, and functional components was improved by optimizing the acidity of extraction solvents, the sequence of ice bath and oscillation, the volumetric solution, and so on. The PRiME HLB SPE pretreatment method was chosen as the optimal one when comparing four pretreatment methods. Among the 65 contaminants, 38 of those determined by liquid chromatography and 41 of those by gas chromatography, which showed good linearity (R² > 0.9801), 97 % of them had a limit of quantitation (LOQ) of lower than 0.02 mg kg^-1. The recovery of all compounds were suited between 70 % to 120 % and the RSD were all lower than 20 % at the spiked levels of LOQ, 2 × LOQ, and 10 × LOQ. For ferulic acid, the LOQ was 50 ng/mL, and it showed good linearity (R²=0.9988) within the range of 0.5 to 10 μg/mL. The recovery and RSD were 98.1 %, and 3.2 % (n = 6), respectively. The simultaneous determination of cross-category compounds in a single sample preparation was obtained by the combination of SPE and GC/LC-Q-TOF/MS. Therefore, this study could not only shorten the time for data acquisition and data analysis, but also improve the experimental efficiency.

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来源期刊

Journal of Chromatography A 化学-分析化学

CiteScore

7.90

自引率

14.60%

发文量

742

审稿时长

45 days

期刊介绍： The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.