摘要本研究建立了一种基质固相分散 （micro-MSPD） 的快速，简单，高效的样品提取方法，从石榴皮中提取多酚。通过与四极飞行时间质谱联用的超高效液相色谱法测定五种目标分析物 （没食子酸，安石榴甙A，安石榴甙B，儿茶素和鞣花酸） 。碳分子筛 （CMS） 作为MSPD分散剂，用于提高样品提取效率。我们研究和优化了分散剂类型，分散剂用量，研磨时间和洗脱溶剂等影响萃取效率的主要参数。在优化条件下，用32。5 mg的CMS分散26 mg石榴皮，研磨时间为90 s，分散的样品用200 μL甲醇洗脱，达到最大提取效率。结果表明，该方法在分析物浓度与峰面积 （相关系数r2> 0。990） 之间具有良好的线性关系，检测限低于3。18 ng/mL，加标回收率在88。06％〜105。71％之间。在石榴皮样品多酚分析中获得了令人满意的结果，证明了该方法的可靠性和高灵敏度。88011

  A rapid, simple and efficient sample extraction method based on micro-matrix-solid-phase dispersion (micro-MSPD) was applied to the extraction of polyphenols from pomegranate peel。 Five target analytes (gallic acid, punicalagin A, punicalagin B, catechin and ellagic acid) were determined by ultra-high-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry。 Carbon molecular sieve (CMS) was used to improve extraction efficiency, which was the first time as the micro-MSPD dispersant in practice。 The major parameters affected extraction efficiency, such as type of dispersant, the amount of dispersant, grinding time and elution solvents, were studied and optimized。 Under optimized conditions, 26 mg of pomegranate peel were dispersed with 32。5 mg of CMS, and the grinding time was 90 s。 The dispersed sample was eluted with 200 μL of methanol to achieve the maximum extraction efficiency。 The results presented that the proposed method was of good linearity between concentrations of analytes and their peak areas (correlation coefficients r2>0。990), and the limit of the detection below 3。18 ng/mL, the spiking recoveries were between 88。06% and 105。71%。 Satisfactory results were obtained in the analysis of polyphenols from pomegranate peel sample, which demonstrated the reliability and high sensitivity of this approach。

毕业论文关键词：碳分子筛; 微基质-固相分散体; 多酚; 石榴果皮; 四极杆飞行时间串联质谱法; 超高效液相色谱

Keyword: Carbon molecular sieve; Micro-matrix-solid-phase dispersion; Polyphenols; Pomegranate peel; Quadrupole time-of-flight tandem mass spectrometry; Ultra-high-performance liquid chromatography 源-于,优W尔Y论L文.网wwW.youeRw.com 原文+QQ75201,8766

目    录

1。引言 6

2。实验 7

2。1 药品试剂 7

2。2 仪器 7

2。3 UAE程序 8

2。4 微MSPD程序 8

3。结果与讨论 8

3。1 CMS的表征 8

3。2 MSPD提取优化 10

3。2。1 分散剂类型 10

3。2。2 分散剂用量 10

3。2。3 研磨时间 11

3。2。4 洗脱溶剂 11

3。3方法评价 12

3。4样品分析 13From~优E尔L论E文W网wWw.YoUeRw.com 加QQ7520.18766

3。5 MSPD-UHPLC-Q-TOF / MS方法与其他方法的比较