【作者】 王洪宇；

【导师】 刘芃岩；

【作者基本信息】 河北大学 ， 分析化学， 2006， 硕士

【摘要】 本学位论文共分两部分。第一部分包括第一、二章，介绍了可食性动物样品中氟喹诺酮类兽药残留的分析方法，并以猪肉为研究对象，SPE-HPLC法对动物固体中多种氟喹诺酮类兽药残留的分析方法进行了系统的研究；第二部分包括第三章，研究了复方制剂养心生脉胶囊中丹参素含量的分析测定方法。具体内容为： 第一章：概括了氟喹诺酮类药物的残留分析测定方法的进展。首先详细介绍了氟喹诺酮分析方法的发展状况，并对现有氟喹诺酮类药物残留检测技术进行了总结，最后介绍了可食性动物样品中氟喹诺酮类药物残留分析的实例。 第二章：以猪肉为研究对象，研究了动物固体样品中多种氟喹诺酮类兽药残留的分析方法。样品以乙腈—冰醋酸为提取剂，经正己烷萃取后，用C₁₈固相萃取小柱快速净化提取物，液相色谱分离检测。该方法线性范围为0.1～10mg／L；检测限为9～14μg／kg；加标回收率为66～92％（RSD＜5％，n=3）。 样品前处理采用溶剂提取、固相萃取净化的方法，首先从常用的提取溶剂中选定醋酸化乙腈作为提取溶剂，然后选择C₁₈固相萃取小柱进行样品净化，最后氮吹浓缩富集。该前处理方法，操作性强，溶剂用量小，分析时间短，样品基质干扰小，加标回收率高。 本文通过实验确定了高效液相色谱——二极管阵列分离检测的分析条件。调节缓冲溶液的组成及有机系和水系的比例，确定流动相的组成，使多种氟喹诺酮类药物得到很好的分离，并以保留时间和最大吸收波长定性各单标药物；采用外标法定量，并对方法的准确度、精密度、线性回归和检测限进行了验证。 该分析方法可同时测定7种氟喹诺酮类药物在动物食品中的残留量，准确度高、精密度好、线性关系良好，检出限低，加标回收率高。 第三章：建立用HPLC-PDA法测定养心生脉颗粒中丹参素含量的方法。色谱条件采用RP₁₈色谱柱；以甲醇-水-冰醋酸为流动相，PDA扫描确定检测波长为280nm。测定结果，丹参素在9.5～152μg／mL范围内，线性关系良好；加标回收率平均为98.9％，RSD为0.97％。为丹参类颗粒的质量综合评价和质量控制提供了简单、准确、可行的分析方法。更多还原

【Abstract】 The thesis consists of two parts. The first part analytical method of fluoroquinolones residues in esculent animals are introduced. In this paper pork is the analytical object and SPE-HPLC methods of determination of fluoroquinolones multiresidues are summarized. In the second part analytical method of determination of salvianolic acid in yangxinshengmai granule is introduced. The details are as following:In Chapter One: actuality and progress technologies of determination of common pharmaceutical fluoroquinolones are summarized. Firstly, introduced progress on analytical method of fluoroquinolones. Secondly, summarized determination technology on fluoroquinolones residues. Finally, showed some examples to introduce how to analyze fluoroquinolones residues in esculent animal samples.In Chapter Two: pork is the analytical object in this paper. The determination of fluoroquinolones multiresidues in solid animal samples are introduced. The samples is extracted by acetonitrile-acetic acid, then extracted by n-hexane,then purified by solid phase extraction C18 cartridge, finally determined by HPLC. The linear range of the method is 0.1～10 mg/L; the detection limit is 9～14 μg/kg; the recovery of the method is 66～92% (RSD<5%, n=3) .The parameters of high performance liquid chromatography (HPLC)-diode array detector (DAD) are confirmed. The mobile phase is confirmed by regulation of the component of buffer solution and the proportion of organic solvent and water, and many fluoroquinolones are separated excellently. Then each fluoroquinolone is determined by retention time and the max absorption wavelength. The external standard method is used, and the accuracy, precision, linear regression, detect limit are validated.The method can be used to determine seven fluoroquinolones in the esculent animal samples at the same time with high accuracy, high precision, good linear relationship and low detect limit.更多还原