摘要本文介绍了使用介孔分子筛KIT-6作为基质固相分散（MMSPD）的吸附剂结合超高效液相色谱来测定黄芩，牙膏和唾液中的植物抗菌素。在这个实验中，首先，KIT-6被用作提取的吸附材料。与一般的硅胶基质吸附剂（C18和硅胶）相比，提出的KIT-6具有三维空间结构和高度有序的介孔排列通道且对待测物质有极好的吸附能力。此外，一些实验变量比如样品和分散剂的质量比，研磨时间，洗脱液的种类被优化来最大的提高提取的效率。提出的分析方法简单，快速，样品消耗量少，分散剂和洗脱剂符合绿色化学的要求，在最优化的条件下，通过分析标准牙膏的三种植物抗菌素的回收率是95.22-101.05%，检出限和分析物的量化分别在0.02–0.04 ng和0.07–0.13 ng的范围内。最后，基质固相微萃取技术成功地被应用在实际样品中的目标溶质分析，并得到了满意的结果。47165

ABSTRACT

This article describes the use of mesoporous molecular sieve KIT-6 as a sorbent in matrix micro solid phase dispersion (MMSPD), together with ultra-performance liquid chromatography, for the determination of plant antibiotics in Scutellariae Radix, toothpaste and saliva. In this study, for the first time, KIT-6 was used as a sorbent material for this mode of extraction. Compared with common silica-based sorbents (C18 and silica gel), the proposed KIT-6 dispersant with a three-dimensional cubic Ia3d structure and highly ordered arrays of mesoporous channels exhibits excellent adsorption capability of tested compounds. In addition, several experimental variables, such as the mass ratio of sample to dispersant, grinding time, and elution solvent, were optimized in order to maximize the extraction efficiency. The proposed analytical method is simple, fast, and entails low consumption of samples, dispersants and elution solvents, meeting “green chemistry” requirements. Under the optimized conditions, the recovery of three herbal antibiotics obtained by analyzing the spiked toothpaste was from 95.22-101.05%. Limits of detection and quantification for determining the analytes were in the range of 0.02–0.04 ng and 0.07–0.13 ng, respectively. Finally, the MMSPD method has been successfully applied to the analysis of target solutes in real samples, and satisfactory results were obtained.

毕业论文关键词：基质固相分散；多空分子筛；植物抗菌素；黄芩；牙膏

Keywords: Matrix micro solid phase dispersion, Mesoporous molecular sieve, Plant antibiotics, Scutellariae Radix, Toothp

目录

1. 引言 5

2.实验部分 6

2.1仪器与药品 6

2.2色谱条件 6

2.3对照品溶液制备过程 6

2.4药典药材样品制备过程 7

2.5唾液样品制备过程 7

2.6牙膏普通提取过程 7

3. 操作过程及结果 7

3.1 KIT-6合成步骤 7

3.2 测试及优化条件 8

3.2.1 考察牙膏与吸附剂之间比例 8

3.2.2研磨时间考察 9

3.2.3考察洗脱液种类 10

3.2.4药材和干燥剂比例考察 11

3.2.5洗脱液体积考察 12

3.2.6考察吸附剂种类 13

3.3标准曲线绘制： 14