Szepesi G
Hnmán Oltóanyagtermelö és Kutató Intézet, Budapest.
Acta Pharm Hung. 1991 Mar;61(2):67-76.
Ruggedness is a measure of the reproducibility of the individual test results when the procedure is used repeatedly to determine the same homogeneous sample in a variety of specified experimental conditions. Ruggedness testing can be divided into two major groups: Type-A, when the influence of the changed environmental conditions (different equipment, analysts, etc.) on the analytical performance parameters and results are tested, and Type-B, when the effect of variation in the experimental conditions are checked. In the latter case, Type-B group can be further classified into two major subgroups: ruggedness testing of sample preparation and chromatographic separation. Checking sample preparation for ruggedness testing includes the investigation of various sample preparation procedures, such as: liquid-liquid extraction, solid phase extraction, direct sample introduction and derivative formation. The investigation of column-to-column variability, changes in the instrumental and experimental conditions belongs to the ruggedness testing of chromatographic separation. In this paper the basic principles of selection for experimental variables for various ruggedness tests are discussed introducing a new possibility to design multivariable-multicriteria system, and the evaluation of a single-variable-single-criterion system, as well. In general, from the work introduced in this paper, it can be concluded that when new analytical methods are developed, it is quite important to be aware the sensitivity of the method to variations in the specified conditions. For adequate performance of ruggedness testing: a) the factors (variables) which have significant influence on the chromatographic results can be firstly selected, b) maximum acceptable deviations from the prespecified experimental conditions can be decided, and c) the acceptable deviations from the values of the prespecified analytical performance parameters can be defined.
耐用性是指当该程序在各种规定的实验条件下反复用于测定同一均匀样品时，各个测试结果的重现性。耐用性测试可分为两大类：A 型，测试环境条件变化（不同设备、分析人员等）对分析性能参数和结果的影响；B 型，检查实验条件变化的影响。在后一种情况下，B 型组可进一步分为两个主要子组：样品制备的耐用性测试和色谱分离的耐用性测试。检查样品制备的耐用性测试包括研究各种样品制备程序，例如：液 - 液萃取、固相萃取、直接进样和衍生化形成。柱与柱之间的变异性研究、仪器和实验条件的变化属于色谱分离的耐用性测试。本文讨论了各种耐用性测试实验变量选择的基本原理，介绍了设计多变量 - 多标准系统的新可能性，以及单变量 - 单标准系统的评估。一般来说，从本文介绍的工作可以得出结论，在开发新的分析方法时，了解该方法对规定条件变化的敏感性非常重要。为了使耐用性测试充分发挥作用：a）可以首先选择对色谱结果有重大影响的因素（变量），b）可以确定与预定实验条件的最大可接受偏差，c）可以定义与预定分析性能参数值的可接受偏差。
