论文总字数：19185字

摘 要

本实验所用的方法原理是氟虫腈（fipronil）在280nm的紫外波长处有吸收，能够通过色谱柱来分离氟虫腈的成分，并对其吸收度的大小作相应的推测。在一定浓度以下，氟虫腈试剂的吸收度会随浓度的上升而上升。

对于不同药物的检测，HPLC法的侧重点与实际要求也会存在一定的差异，例如，在使用HPLC法进行杂质定量试验或者鉴别试剂时，专属性就是其鉴别侧重点。因此需要检测试验中所采用的HPLC法是否满足试验中具体所规定的范围标准，从而证明HPLC的可行性与适用性。为了确定所使用的用来检测氟虫腈的HPLC法所需条件的准确性与可靠性，通常可采用方法学验证其对氟虫腈的适用性和准确可靠性，而HPLC法所需要验证的实验通常包含系统残留实验，特异性实验，系统适应性实验，准确度与精密度（批间精密度与批内精密度）实验，均匀性实验，稳定性（储备液及供试品稳定性）试验等实验项目。通过空白溶液与储备液分别进样的图谱可以看出系统残留以及特异性均满足要求。准确度与精密度的实验证明了系统精确度高，试验方法正确。均匀性实验证明了配制的溶液符合要求。稳定性实验证明了配制的溶液稳定。综上本次试验比较完整的对氟虫腈原药HPLC的方法进行了研究。对氟虫腈的主成分及其杂质的相关研究具有一定的实际生产价值。

关键词：氟虫腈；分析方法学；高效液相色谱法

Methodology Research On Determination of fipronil

Abstract

Method principle is used in this study fipronil had absorption in the uv wavelength of 280 nm, can take advantage of the chromatographic column of fipronilcomponent separation, and speculated that the size of the absorbance.In a certain concentration range, the absorbance of fluorine worm cyanide reagent and its concentration is proportional to the.

HPLC method in the detection of different drugs with different actual requirements or focus, such as adopting HPLC method for preparation of identification and impurities quantitative experiment, the preparation of specificity to identify key requirements.So it is necessary to HPLC method adopted by the test whether meet the test standard in the range of specific regulations, so as to prove feasibility and applicability of HPLC.In order to determine the use of HPLC method used to detect fluoride insect nitrile accuracy and reliability of the required conditions, generally, the methodology can be used to verify its reliability, applicability and accuracy of fiproniland HPLC to the methodology validation experiment contents mainly include system suitability testing, specific experiment, the system residual test, accuracy and precision (precision) in precision between batch and batch experiments, homogeneity test, stability test (stock solution and the stability of the test), etc. The experiment project.。The residual and specificity of the system can be met by the injection of the blank solution and the reserve liquid.. The accuracy and accuracy of the experiments are proved to have the accuracy of the system and the method of the test is correct.. The uniformity experiment proved the solution to meet the requirement.. The stability of the solution is proved by the stability experiment.. The method of Fipronil in the HPLC after the test is complete is studied. The study of the main components and impurities of the main components of the fluorine has some practical value for production..

Keywords: Fipronil; Analysis Methodology; HPLC

目 录

摘 要 I

Abstract II

第一章 引 言 1

1.1 氟虫腈概述 1

1.2 研究背景 1

1.3 高效液相色谱介绍 2

1.3.1HPLC法在鉴别药物中的运用 2

1.3.2HPLC法在杂质鉴定中的运用与特征 3

1.3.3HPLC法在含量检测中的运用 3

第二章 HPLC含量与相关物质测定 4

2.1 验证对象 4

2.2 目 的 4

2.3 参考文件 4

2.4 验证内容 4

2.5 主要试剂和仪器 5

2.6色谱条件 6

2.7 对照储备液的制备 6

2.8 标准溶液的制备 7

2.9 供试品的制备 7

第三章 方法学验证 8

3.1 特异性 8

3.2 系统残留 8

3.3 标准曲线 8

3.4 准确度 8

3.5 精密度 8

3.6 均匀性 9

3.7 稳定性 9

第四章 验证结果与讨论 10

4.1 特异性 10

4.2 系统残留 10

4.3 储备液 10

4.4 标准曲线 11

4.5 精密度 15

4.6 灵敏度 15

4.6.1 定量限(LOQ) 15

4.6.2 检测限(LOD) 16

4.7 均一性 16

4.8 稳定性 17

第五章 结 论 18

致 谢 19

参考文献（Refrences） 20

第一章 引 言

1.1 氟虫腈概述

氟虫腈^[1]也称作氟苯唑、锐劲特、Regent、Phenylpyrazoles、Icon、Frontline、Fipronil等，其化学名为(±)-5-氨基-1-(2,6-二氯-α,α,α-三氟-p-甲苯基-)-4-三氟甲基-3-氰基吡唑-亚硫酰基，化学结构式如下图所示：

图1.1氟虫腈结构式

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