USP-1092-溶出度试验的开发和验证(中英文对照版)

溶出度试验的开发和验证INTRODUCTION前言Purpose目的The Dissolution Procedure: Developmentand Validation <1092> provides a comprehensive approach covering items to considerfor developing and validating dissolution procedures and the accompanyinganalytical procedures、It addresses the use of automation throughout the testand provides guidance and criteria for validation、 It also addresses thetreatment of the data generated and the interpretation of acceptance criteriafor immediate- and modified-release solid oral dosage forms、溶出实验:开发与验证(1092)指导原则提供了在溶出度方法开发与验证过程中以及采用相应分析方法时需要考虑的因素。

本指导原则贯穿溶出度实验的全部过程,并对方法提供了指导与验证标准。

同时它还涉及对普通制剂与缓释制剂所生成的数据与接受标准进行说明。

Scope范围Chapter <1092> addresses the development andvalidation of dissolution procedures, with a focus on solid oral dosage forms、Many of the concepts presented, however, may be applicable to other dosageforms and routes of administration、General recommendations are given with theunderstanding that modifications of the apparatus and procedures as given in USP general chapters need to be justified、<1092>章节讨论了溶出度实验的开发与验证,重点就是口服固体制剂。

INTRODUCTION前言Purpose目的The Dissolution Procedure: Developmentand Validation <1092> provides a comprehensive approach covering items to considerfor developing and validating dissolution procedures and the accompanyinganalytical procedures. It addresses the use of automation throughout the testand provides guidance and criteria for validation. It also addresses thetreatment of the data generated and the interpretation of acceptance criteriafor immediate- and modified-release solid oral dosage forms.溶出实验:开发和验证（1092）指导原则提供了在溶出度方法开发和验证过程中以及采用相应分析方法时需要考虑的因素。

本指导原则贯穿溶出度实验的全部过程，并对方法提供了指导和验证标准。

同时它还涉及对普通制剂和缓释制剂所生成的数据和接受标准进行说明。

Scope围Chapter <1092> addresses the development andvalidation of dissolution procedures, with a focus on solid oral dosage forms.Many of the concepts presented, however, may be applicable to other dosageforms and routes of administration. General recommendations are given with theunderstanding that modifications of the apparatus and procedures as given in USP general chapters need to be justified.<1092>章节讨论了溶出度实验的开发和验证，重点是口服固体制剂。

溶出度方法验证浅析摘要：根据美国药典<1092>章节溶出度方法的开发和验证，结合FDA、ICH指南和中国药典方法验证指导原则，对溶出度方法验证需要研究的项目、操作要求和认可标准进行了探讨。

关键词：溶出度；方法验证Validation of dissolution procedureHuang Fengming (Zhejiang Hisun Animal Healthcare pharmaceutical (Hangzhou) Co., Ltd, Hangzhou 311400)ABSTRACT: Discussed the validation characteristics, operation requirements and acceptance criteria for dissolution procedure according to USP <1092> general chapter combined with FDA and ICH guidelines and ChP general chapter.KEY WORDS: dissolution, method validation关于分析方法验证相关指南在以下文献中有描述：中国药典2020年版附录9101[1]、美国药典通则<1225> Validation of Compendial Procedure[2]、FDA工业指南：Analytical Procedures and Methods Validation for Drugs and Biologics[3]、ICHQ2: VALIDATION OF ANALYTICAL PROCEDURES: TEXT AND METHODOLOGY[4]。

由于溶出度分析方法验证对制剂样品质量要求比较高，例如含量均匀度要求窄，溶出行为均一，在使用到制剂样品的验证项目中需要特别注意，制剂样品质量会成为影响溶出度分析方法验证成败的关键。

圣诞礼物 一致性评价重磅参考资料：（USP1092）溶出度试验的开发和验证（续）2015­12­25刘建华医药信息新药开发3.分析整理溶出步骤也是一个复杂的样品制备过程。

用于测定溶出过程中药物溶出量的处理和分析过程，称为“分析整理”。

虽然本章讨论的分光光度法和高效液相色谱法是最常用的分析方法，其他适宜的分析技术也可以使用。

在第5节，将详细描述方法验证标准。

3.1 样品处理溶出样品在取样后，需要进一步的处理，使能够满足样品释放量的分析方法的测定要求。

例如，过滤可用于除去未溶解的颗粒物样品，或者避光、冷藏贮存样品。

此外，样品可能需要稀释至方法线性范围内的测定浓度。

使用高效液相色谱法时，尽可能采用流动相稀释至样品以减少溶出介质对样品测定的影响。

根据产品特性的要求，其他类型的处理方式也是存在的。

例如加入适当的试剂使产生干扰的物质消除或者失活。

然而，分离可能是不可能的或需要的不是必需的，在一些情况下，在原位测量的方法，如纤维光学或电化学测定方法可能是有用的。

3.2 过滤在上面1.1章节中已经讲述。

3.3 离心离心处理样品是不优选的，具体原因有以下几个方面：在固体颗粒除去之前，药物溶解可以继续发生，是药物的溶出浓度增大，并且离心的动力也可能导致增加溶解的药物颗粒。

然而当所有常见滤膜对药物均有吸附或者所有滤膜均干扰药物的测定时（例如，使用荧光定量），可以选择离心法处理样品。

离心法可以证明是有用的，在方法开发的过滤材料的适用性评价。

3.4 分析方法用于溶出度测定的常用分析方法一般为分光光度法或液相色谱法。

分光光度法较高效液相法更简便快捷，并且分光光度法较HPLC法更容易自动化，并且溶剂量使用较少。

但是分光光度法测定需要专属性良好。

高效液相色谱法是首选的原因有很多，如提供较宽测定范围，减少了需要稀释样品的步骤，提高了低浓度样品的分析灵敏度，并且可用于辅料或者多组分互相干扰的样品的测定。

目前的高效液相色谱系统采用自动进样器，提高了自动化。

VALIDATION OF COMPENDIAL PROCEDURES 药典方法的验证Test procedures for assessment of the quality levels of pharmaceutical articles are subject to various requirements. According to Section 501 of the Federal Food, Drug, and Cosmetic Act, assays and specifications in monographs of the United States Pharmacopeia and the National Formulary constitute legal standards. The Current Good Manufacturing Practice regulations [21 CFR 211.194(a)] require that test methods, which are used for assessing compliance of pharmaceutical articles with established specifications, must meet proper standards of accuracy and reliability. Also, according to these regulations [21 CFR 211.194(a)(2)], users of analytical methods describedin USP–NF are not required to validate the accuracy and reliability of these methods, but merely verify their suitability under actual conditions of use. Recognizing the legal status of USP and NF standards, it is essential, therefore, that proposals for adoption of new or revised compendial analytical procedures be supported by sufficient laboratory data to document their validity.用于评估药品质量的检验方法需要满足不同的要求。

（ 1092）溶出度试验的开发和验证【中英文对照版】INTRODUCTION前言Purpose目的The Dissolution Procedure: Developmentand Validation<1092>provides a comprehensive approach covering items to considerfor developing and validating dissolutionprocedures and the accompanyinganalytical procedures. Itaddresses the use of automation throughout the testandprovides guidance and criteria for validation.It also addresses thetreatment of the data generated and the interpretationof acceptance criteriafor immediate-and modified-releasesolid oral dosage forms.溶出实验:开发和验证（1092）指导原则提供了在溶出度方法开发和验证过程中以及采用相应分析方法时需要考虑的因素。

本指导原则贯穿溶出度实验的全部过程，并对方法提供了指导和验证标准。

同时它还涉及对普通制剂和缓释制剂所生成的数据和接受标准进行说明。

Scope范围Chapter<1092>addresses the development andvalidationof dissolution procedures,with a focus on solid oral dosage forms.Many of the concepts presented, however, may beapplicable to other dosageforms and routes of administration. General recommendations are given with theunderstandingthat modifications of the apparatus and procedures as given in USP general chapters need to be justified.<1092>章节讨论了溶出度实验的开发和验证，重点是口服固体制剂。

INTRODUCTION前言Purpose目的The Dissolution Procedure: Developmentand Validation <1092> provides a prehensive approach covering items to considerfor developing and validating dissolution procedures and the acpanyinganalytical procedures. It addresses the use of automation throughout the testand provides guidance and criteria for validation. It also addresses thetreatment of the data generated and the interpretation of acceptance criteriafor immediate- and modified-release solid oral dosage forms.溶出实验:开发和验证〔1092〕指导原那么提供了在溶出度方法开发和验证过程中以及采用相应分析方法时需要考虑的因素。

本指导原那么贯穿溶出度实验的全部过程，并对方法提供了指导和验证标准。

同时它还涉及对普通制剂和缓释制剂所生成的数据和承受标准进展说明。

Scope围Chapter <1092> addresses the development andvalidation of dissolution procedures, with a focus on solid oral dosage forms.Many of the concepts presented,however, may be applicable to other dosageforms and routes of administration. General remendations are given with theunderstanding that modifications of the apparatus and procedures as given in USP general chapters need to be justified.<1092>章节讨论了溶出度实验的开发和验证，重点是口服固体制剂。

（1092）溶出度实验的开发和验证【中英文对照版】INTRODUCTION前言Purpose目的The Dissolution Procedure: Developmentand Validation <1092> provides a comprehensive approach covering items to considerfor developing and validating dissolution procedures and the accompanyinganalytical procedures. It addresses the use of automation throughout the testand provides guidance and criteria for validation. It also addresses thetreatment of the data generated and the interpretation of acceptance criteriafor immediate- and modified-release solid oral dosage forms.溶出实验:开发和验证（1092）指导原则提供了在溶出度方法开发和验证过程中以及采用相应分析方法时需要考虑的因素。

本指导原则贯穿溶出度实验的全部过程，并对方法提供了指导和验证标准。

同时它还涉及对普通制剂和缓释制剂所生成的数据和接受标准进行说明。

Scope范围Chapter <1092> addresses the development andvalidation of dissolution procedures, with a focus on solid oral dosage forms.Many of the concepts presented, however, may be applicable to other dosageforms and routes of administration. General recommendations are given with theunderstanding that modifications of the apparatus and procedures as given in USP general chapters need to be justified.<1092>章节讨论了溶出度实验的开发和验证，重点是口服固体制剂。

（ 1092）溶出度试验的开发和验证【中英文对照版】INTRODUCTION前言Purpose目的The Dissolution Procedure: Developmentand Validation<1092>provides a comprehensive approach covering items to considerfor developing and validating dissolutionprocedures and the accompanyinganalytical procedures. Itaddresses the use of automation throughout the testandprovides guidance and criteria for validation.It also addresses thetreatment of the data generated and the interpretationof acceptance criteriafor immediate-and modified-releasesolid oral dosage forms.溶出实验:开发和验证（1092）指导原则提供了在溶出度方法开发和验证过程中以及采用相应分析方法时需要考虑的因素。

本指导原则贯穿溶出度实验的全部过程，并对方法提供了指导和验证标准。

同时它还涉及对普通制剂和缓释制剂所生成的数据和接受标准进行说明。

Scope范围Chapter<1092>addresses the development andvalidationof dissolution procedures,with a focus on solid oral dosage forms.Many of the concepts presented, however, may beapplicable to other dosageforms and routes of administration. General recommendations are given with theunderstandingthat modifications of the apparatus and procedures as given in USP general chapters need to be justified.<1092>章节讨论了溶出度实验的开发和验证，重点是口服固体制剂。