Key Laboratory of Flexible Electronics & Institute of Advanced Materials, Jiangsu National Synergetic Innovation Center for Advanced Materials, Nanjing Tech University, Nanjing, P. R. China.
Institute of Quality and Standards for Agricultural Products, Zhejiang Academy of Agricultural Sciences, Hangzhou, P. R. China.
J Sep Sci. 2020 Apr;43(8):1558-1565. doi: 10.1002/jssc.201900900. Epub 2020 Mar 12.
A high-throughput and environmentally friendly method based on 96-well plate thin-film microextraction was established to determine 14 fungicides in grapes and grape juice using liquid chromatography-tandem mass spectrometry. The thin-film microextraction optimized method consisted of 60 min of extraction at pH 6.0 with the addition of sodium chloride (2-5%). Acetonitrile/water in the ratio of 8:2 was used for desorption analytes for 60 min. Evaluation of different extractive phases showed that polyacrylonitrile-polystyrene-divinylbenzene was the optimum coating. The linearity of the method was good in the range of 0.01-0.5 μg/mL for 14 fungicides with determination coefficients (R ) from 0.990 to 0.999, which indicated good linearity for both the grape juice and grape matrixes. The limit of detection was in the range of 0.002-0.01 μg/mL. The limit of quantitation was in the range of 0.01 mg/kg according to the minimum fortified level. The average absolute recoveries of the 14 fungicides ranged from 75.0 to 118.3%. The intraday relative standard deviation (n = 4) and interday relative standard deviation (n = 4) were 5.6-13.0% and 1.6-6.4%, respectively. This study showed that this method can be used for analyzing 96 samples in parallel, and the sample preparation time was approximately 2.0 min per sample. In addition, this approach offers a green and low-cost sample pretreatment technique for future analyses.
基于 96 孔板薄膜微萃取，建立了一种高通量且环境友好的方法，用于使用液相色谱-串联质谱法测定葡萄和葡萄汁中的 14 种杀菌剂。薄膜微萃取优化方法包括在 pH 6.0 下加入氯化钠（2-5%）萃取 60 分钟。用乙腈/水（8:2）解吸分析物 60 分钟。评价不同的萃取相表明，聚丙烯腈-聚苯乙烯-二乙烯基苯是最佳的涂层。该方法在 0.01-0.5μg/mL 范围内对 14 种杀菌剂具有良好的线性，决定系数（R ）在 0.990-0.999 之间，表明该方法对葡萄汁和葡萄基质均具有良好的线性。检出限在 0.002-0.01μg/mL 范围内。根据最小加标水平，定量限在 0.01mg/kg 范围内。14 种杀菌剂的平均绝对回收率在 75.0-118.3%之间。日内相对标准偏差（n=4）和日间相对标准偏差（n=4）分别为 5.6-13.0%和 1.6-6.4%。该研究表明，该方法可用于同时分析 96 个样品，每个样品的样品制备时间约为 2.0 分钟。此外，该方法为未来的分析提供了一种绿色且低成本的样品预处理技术。
