Validation of analytical methods: the international requirements

2018 ◽  
Vol 84 (12) ◽  
pp. 25-31
Author(s):  
V. B. Baranovskaya ◽  
M. Yu. Medvedevskikh
Keyword(s):  
Analytical Chemistry ◽  
Chemical Analysis ◽  
Analytical Method ◽  
Analytical Methods ◽  
Metrological Certification ◽  
Metrological Characteristics ◽  
Fitness For Purpose ◽  
Validation And Verification ◽  
Development And Validation

Analytical method is the most important part of chemical analysis, an action guide for the analyst and carrier of information about the metrological characteristics. To confirm the parameters and legitimize the methodology, Russian specialists traditionally use the procedure of metrological certification in accordance with GOST 8.563-2009. Validation of analytical procedures or analytical methods is a concept recently accepted in Russia and causes confusion in many domestic experts. However, this internationally accepted concept is actively used for long to assure the quality of chemical analysis. The European Community for Metrology in Analytical Chemistry (Eurachem) has developed a guide to validation of analytical methods «The Fitness for Purpose of Analytical Methods»; many articles have been published on this issue. This article is devoted to generalization of the similar features and individual differences in certification, validation and verification of the methods of chemical analysis. Metrological characteristics of the analytical methods are also considered. An emphasis is made on the procedure of estimating the uncertainty as the most important stage in the development and validation of the analytical method.

scholarly journals Comprehensive Assessment of Flow and Other Analytical Methods Dedicated to the Determination of Zinc in Water

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3914
Author(s):  
Paweł Kościelniak ◽  
Paweł Mateusz Nowak ◽  
Joanna Kozak ◽  
Marcin Wieczorek
Keyword(s):  
Analytical Chemistry ◽  
Green Chemistry ◽  
Analytical Method ◽  
Analytical Methods ◽  
Green Analytical Chemistry ◽  
General Quality ◽  
Analytical Strategies ◽  
High Degree

An original strategy to evaluate analytical procedures is proposed and applied to verify if the flow-based methods, generally favorable in terms of green chemistry, are competitive when their evaluation also relies on other criteria. To this end, eight methods for the determination of zinc in waters, including four flow-based ones, were compared and the Red–Green–Blue (RGB) model was exploited. This model takes into account several features related to the general quality of an analytical method, namely, its analytical efficiency, compliance with the green analytical chemistry, as well as practical and economic usefulness. Amongst the investigated methods, the best was the flow-based spectrofluorimetric one, and a negative example was that one involving a flow module, ICP ionization and MS detection, which was very good in analytical terms, but worse in relation to other aspects, which significantly limits its overall potential. Good assessments were also noted for non-flow electrochemical methods, which attract attention with a high degree of balance of features and, therefore, high versatility. The original attempt to confront several worldwide accepted analytical strategies, although to some extent subjective and with limitations, provides interesting information and indications, establishing a novel direction towards the development and evaluation of analytical methods.

scholarly journals Implementing Green Analytical Methodologies Using Solid-Phase Microextraction: A Review

Molecules ◽  
2020 ◽  
Vol 25 (22) ◽  
pp. 5297
Author(s):  
Kayla M. Billiard ◽  
Amanda R. Dershem ◽  
Emanuela Gionfriddo
Keyword(s):  
Analytical Chemistry ◽  
Sample Preparation ◽  
Analytical Method ◽  
Analytical Methods ◽  
Solid Phase Microextraction ◽  
Method Development ◽  
Assessment Tool ◽  
Solid Phase ◽  
Assessment Tools ◽  
Green Analytical Chemistry

Implementing green analytical methodologies has been one of the main objectives of the analytical chemistry community for the past two decades. Sample preparation and extraction procedures are two parts of analytical method development that can be best adapted to meet the principles of green analytical chemistry. The goal of transitioning to green analytical chemistry is to establish new methods that perform comparably—or superiorly—to traditional methods. The use of assessment tools to provide an objective and concise evaluation of the analytical methods’ adherence to the principles of green analytical chemistry is critical to achieving this goal. In this review, we describe various sample preparation and extraction methods that can be used to increase the greenness of a given analytical method. We gave special emphasis to modern microextraction technologies and their important contributions to the development of new green analytical methods. Several manuscripts in which the greenness of a solid-phase microextraction (SPME) technique was compared to other sample preparation strategies using the Green Analytical Procedure Index (GAPI), a green assessment tool, were reviewed.

Automation and Quality in Analytical Laboratories

1994 ◽  
Vol 77 (3) ◽  
pp. 785-789
Author(s):  
Miguel Valcárcel ◽  
Angel Ríos
Keyword(s):  
Analytical Chemistry ◽  
Quality Control ◽  
Chemical Analysis ◽  
Analytical Control ◽  
Systems Quality ◽  
Quality Of Products ◽  
Analytical Laboratories

Abstract After a brief introduction to the generic aspects of automation in analytical laboratories, the different approaches to quality in analytical chemistry are presented and discussed to establish the following different facets emerging from the combination of quality and automation: automated analytical control of quality of products and systems; quality control of automated chemical analysis; and improvement of capital (accuracy and representativeness), basic (sensitivity, precision, and selectivity), and complementary (rapidity, cost, and personnel factors) analytical features. Several examples are presented to demonstrate the importance of this marriage of convenience in present and future analytical chemistry.

A Technique for the Objective Assessment of Routine Analytical Methods in Clinical Laboratories Using Pattern Recognition

1981 ◽  
Vol 18 (4) ◽  
pp. 218-225 ◽  
Author(s):  
Rob T P Jansen ◽  
F W Pijpers ◽  
G A J M De Valk
Keyword(s):  
Pattern Recognition ◽  
Analytical Method ◽  
Analytical Methods ◽  
Dimensional Space ◽  
Objective Assessment ◽  
Control Programme ◽  
Internal Quality ◽  
Bias Drift ◽  
Clinical Laboratories

A technique is presented to assess objectively the reliability of analytical methods used routinely in clinical laboratories. From the Netherlands National Coupled External/Internal Quality Control Programme information can be gathered about the performance of routine analytical methods. The performance of a method in a trial is described by four ‘features’: the accuracy of a method; its day to-day precision; its susceptibility to give erroneous results (eg, extreme bias, drift, extreme week-to-week variations); and its susceptibility to give systematic errors for different laboratories. These four features obtained in a trial for a given analytical method determine the position of a ‘pattern’ in the four-dimensional space. The results of six trials discussed in this paper provided six ‘patterns' per analytical method. Using pattern recognition techniques, clusters of patterns were detected in the four-dimensional space. A weighting procedure revealed the relative importance of the various features for discrimination between the detected clusters. For various blood components, different features are of importance for this discrimination. Patterns belonging to the same clusters appeared to be patterns of the same (or comparable) analytical methods; thus analytical methods could be distinguished from each other. The means of the feature values of the patterns in a cluster determine the quality of that cluster. Thus the quality of an analytical method can be objectively assessed. Some tentative conclusions on the validity of analytical methods are given.

scholarly journals COLLABORATIVE TRIAL AND QUALITY CONTROL IN CHEMICAL ANALYSIS

2010 ◽  
Vol 2 (3) ◽  
pp. 135-141
Author(s):  
Narsito Narsito
Keyword(s):  
Quality Control ◽  
Chemical Analysis ◽  
Analytical Method ◽  
Control Charts ◽  
Analytical Data ◽  
Control Program ◽  
Quality Parameter ◽  
Quality Control Program ◽  
And Control

Abstract                                                             This paper deals with some practical problems related to the quality of analytical chemical data usually met in practice. Special attention is given to the topic of quality control in analytical chemistry, since analytical data is one of the primary information from which some important scientifically based decision are to be made. The present paper starts with brief description on some fundamental aspects associated with quality of analytical data, such as sources of variation of analytical data, criteria for quality of analytical method, quality assurance in chemical analysis. The assessment of quality parameter for analytical method like the use of standard materials as well as standard methods is given. Concerning with the quality control of analytical data, the use of several techniques, such as control samples and control charts, in monitoring analytical data in quality control program are described qualitatively.  In the final part of this paper, some important remarks for the preparation of collaborative trials, including the evaluation of accuracy and reproducibility of analytical method are also given Keywords: collaborative trials, quality control, analytical data Abstract                                                             This paper deals with some practical problems related to the quality of analytical chemical data usually met in practice. Special attention is given to the topic of quality control in analytical chemistry, since analytical data is one of the primary information from which some important scientifically based decision are to be made. The present paper starts with brief description on some fundamental aspects associated with quality of analytical data, such as sources of variation of analytical data, criteria for quality of analytical method, quality assurance in chemical analysis. The assessment of quality parameter for analytical method like the use of standard materials as well as standard methods is given. Concerning with the quality control of analytical data, the use of several techniques, such as control samples and control charts, in monitoring analytical data in quality control program are described qualitatively.  In the final part of this paper, some important remarks for the preparation of collaborative trials, including the evaluation of accuracy and reproducibility of analytical method are also given Keywords: collaborative trials, quality control, analytical data

Method Validation

2007 ◽  
Author(s):  
D. Brynn Hibbert
Keyword(s):  
Chemical Analysis ◽  
Method Validation ◽  
Analytical Method ◽  
Standard Operating Procedure ◽  
Fitness For Purpose ◽  
Objective Evidence ◽  
Validation Parameters ◽  
American Society ◽  
Potential Methods ◽  
Quality Assurance Method

Many aspects of a chemical analysis must be scrutinized to ensure that the product, a report containing the results of the analysis, fulfills the expectations of the client. One of the more fundamental factors is the analytical method itself. How was it chosen? Where does it come from? When a laboratory is faced with a problem requiring chemical analysis, there may be set methods described in a standard operating procedure, but often the analyst might have to make a choice among methods. For the majority of analytical methods used in field laboratories, there is neither the expertise nor the inclination to start from scratch and reinvent the wheel. The analyst wants a method that can be implemented in his or her laboratory. Compilations of methods that have been evaluated do exist and have the imprimatur of international organizations such as the International Organization for Standardization (ISO) or the American Society for Testing and Materials (ASTM). Failing this, the scientific literature abounds in potential methods that have the recommendation of the authors, but may not always be as suitable as claimed. This chapter has two aims: to demonstrate the necessity of using properly validated and verified methods and to explain what constitutes a validated method, and to provide an introduction to method validation for in-house methods. There is an abundance of published material that defines, describes, and generally assists with method validation, some of which is referenced here (Burgess 2000; Christensen et al. 1995; EURACHEM 1998; Fajgelj and Ambrus 2000; Green 1996; Hibbert 2005; ICH 1995, 1996; LGC 2003; Thompson et al. 2002; USP 1999; Wood 1999). “Method validation” is a term used for the suite of procedures to which an analytical method is subjected to provide objective evidence that the method, if used in the manner specified, will produce results that conform to the statement of the method validation parameters. Like many aspects quality assurance, method validation is of a relative nature. As with the concept of fitness for purpose, a method is validated for a particular use under particular circumstances. If those circumstances vary, then the method would need to be re-validated at least for the differences.

Development and Validation of a Robust HPLC Method for Simultaneous Estimation of 5-Fluorouracil and Resveratrol and Its Application in the Engineered Nanostructured Lipid Carrier

2020 ◽  
Vol 16 ◽  
Author(s):  
Mohammad Kashif Iqubal ◽  
Abid Kamal ◽  
Ashif Iqubal ◽  
Mohammad Imran ◽  
Javed Ali ◽  
...  
Keyword(s):  
Combination Therapy ◽  
Analytical Method ◽  
Analytical Methods ◽  
Mobile Phase ◽  
Cost Effective ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Nanostructured Lipid Carrier ◽  
Development And Validation ◽  
Ich Guideline

Background: 5-fluorouracil and resveratrol are the two most effective anticancer drugs. Combination therapy with these two drugs has shown promising results in cancer. The formulation containing 5-fluorouracil and resveratrol has been prepared, but no analytical method is available in the literature for their simultaneous estimation. However, several analytical methods are there for estimation of either 5-fluorouracil or resveratrol alone. Therefore, the present article is designed for the simultaneous estimation of 5-fluorouracil and resveratrol by HPLC and its application in the quantification of the drugs present in the formulated nanostructured lipid carrier (NLC). Methods: The method was developed using a C18 column (Purospher® STAR RP-18 endcapped (5 µm) Hibar® RT 250- 4.6) with acetonitrile and water as the mobile phase (25:75 v/v) and estimated at 272 nm. The currently developed method was further validated by the ICH guideline Q2 (R1). Combinatorial NLC of 5-fluorouracil and resveratrol was also prepared and characterized. Results: The LOD and LOQ were 8.22 and 24.91 µg mL-1 and 6.58 and 19.93 µg mL-1 , respectively. The precisions was under the acceptable limits of < 2% RSD. The content of 5-fluorouracil and resveratrol in NLC were found to be 65.558±1.343% and 96.326±1.421%, respectively. Conclusion: The findings showed that the developed and validated method was simple, fast, cost-effective and reproducible for the simultaneous estimation of both the drugs in the same formulation.

scholarly journals Quality and Reliability in Analytical Chemistry

Proceedings ◽  
2020 ◽  
Vol 55 (1) ◽  
pp. 8
Author(s):  
Raluca-Ioana Stefan-van Staden
Keyword(s):  
Analytical Chemistry ◽  
Analytical Methods ◽  
Good Practice ◽  
Reliability Evaluation ◽  
New Method ◽  
Undergraduate Studies ◽  
Analytical Information ◽  
Quality And Reliability

Quality and reliability are essential terms in analytical chemistry. Reliable analytical information implies quality. Maintaining the quality in time shows reliability. Evaluation of quality and reliability is essential for the validation of a new method of analysis. Learning good practice in analytical chemistry during undergraduate studies will improve the quality of the laboratories of analysis, by implementing highly reliable analytical methods.

Green analytical solutions for sample preparation: solid phase microextraction and related techniques

2020 ◽  
Vol 5 (8) ◽  
Author(s):  
Emanuela Gionfriddo
Keyword(s):  
Analytical Chemistry ◽  
Sample Preparation ◽  
Analytical Method ◽  
Analytical Methods ◽  
Solid Phase Microextraction ◽  
Method Development ◽  
Solid Phase ◽  
Green Analytical Chemistry ◽  
Chemistry Community

AbstractFor at least three decades, the analytical chemistry community is striving to apply the principles of Green Chemistry to the development of analytical methods. Many efforts have been made to outline the concept of Green Analytical Chemistry, which helped to redefine analytical procedures and drastically changed the philosophy of analytical method development. This book chapter describes the 12 principles of Green Analytical Chemistry and various methodologies for the assessment of the greenness of analytical methods. The three main steps in the analytical method development – sample preparation, separation and detection- are described in a “green perspective”. Special emphasis is given to the description of green sample preparation procedures, in particular to Solid Phase Microextraction, that, since its introduction in 1989 by Janusz Pawliszyn, has drastically revolutionized the methodology of sample preparation, providing a convenient and green alternative to already existing methods.

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