Analytical methods documentation

Analytical method the complete process used to determine an analyte or analytes in a sample. The analytical method documents all the individual steps in the process from sampling to reporting the results. 

The EPA publishes Series Methods that describe the exact procedures to be followed with respect to sample receipt and handling, analytical methods, data reporting, and document control. These guidelines must be followed closely to ensure accuracy, reproducibility, and reliability within and among the contract laboratories. 

The level of quahty required in a LIMS is related to the particular role played by the system in the organi2ation s business. In an R D environment, for example, the primary reason for a LIMS might be to compare and document new analytical methods. 

For those suppliers not conforming to Ford, General Motors, and Daimler Ghrylser requirements, other analytical methods and acceptance criteria may be used if approved by the customer. If you lack any documented methods, the MSA Reference Manual is recommended. 

Some internationally harmonized guidelines regarding specifications and tests, impurities and validation of analytical methods have particular relevance to the development of chiral drugs and are discussed below. In addition, the impact of work on the common technical document is considered. 

Hi) Specialized Analytical Methods. Analytical methods for metallic impurities are well documented and are not covered here. A major advance in the continuous monitoring of impurities in liquid sodium down to the lowest levels of detection has been the development of analysis using electrochemical cells. Oxygen analysis in sodium may be carried out using a cell of the type... 

Standard operating procedures (SOPs)— The SOPs are controlled in a way similar to that of specification documents and analytical methods. It must be ensured that the correct versions of the SOPs are accessed and used by the scientists. After use, the hard copies should be destroyed and disposed of properly. An added requirement is that the SOPs should be accessible during working hours without interruption. Hard copies should be available at a manageable location so that the SOPs are available when the electronic system is down. 

Traditional analytical methods make extensive use of computers, but typically these methods still require constant restructuring of the data and multiple analytical tools. This endless restructuring wastes time and productivity and also makes the analytical processes difficult to document, audit, and reproduce in real time. This situation also makes it difficult to reconstruct and update analyses in real time when new adverse event data become available or when new questions need to be asked. The application of comprehensive data standards allows the use of integrated, reusable software for analyzing adverse event data. This integration facilitates the reproducibility of the results. 

Commission Directive 96/46/EC of 16 July 1996, amending Annex II to the Directive 91/414/EEC, is the basis for the assessment of residue analytical methods for crops, food, feed, and environmental samples." Provisions of this Directive cover methods required for post-registration control and monitoring purposes but not data generation methods. Because it is necessary to provide applicants as precisely as possible with details on the required information, the guidance document S ANCO/825/00 rev. 6 dated 20 June 2000 (formerly 8064/VI/97 rev. 4, dated 5 December 1998)" was elaborated by the Commission Services in cooperation with the Member States. 

Moreover, this document provides guidance to Member States on the interpretation of the provisions of Directive 96/46/EC concerning minimum validation requirements for residue analytical methods. 

For analytical methods used for generating data required in the field of residue behavior, environmental fate, and other fields, the guidance document SANCO/3029/99 rev. 4 was developed."... 

Reliable residue data are generated during the development of an a.i. to support the assessment of the consumer risk (residue data and toxicological data) and the impact on the environment (fate and behavior, efficacy and ecotoxicological data). It is critical that these analytical methods are reliably validated. In the guidance document SANCO/3029/99 rev. 4 (11/07/00), harmonized requirements for the residue analytical method are described. Validated analytical methods are required for the following studies ... 

European Commission, Guidance Document on Residue Analytical Methods, SANCO/ 825/00/rev. 6, 20.06.00. European Commission, Bmssels (2000). This guidance document and also the following ones are available on the World Wide Web http //europa.eu.int/comm/ food/fs/ph ps/pro/wrkdoc/index en.htm. 

Until 1991, manufacturers seeking authorizations for pesticides had to fulfil country-specific requirements of validation of enforcement methods. The term enforcement method means analytical methods which are developed for post-registration control and monitoring purposes. The harmonization of these requirements was initiated with the European Economic Community (EEC) Council Directive 91/414/EEC and temporarily finalized with the Guidance Document on Residue Analytical Methods SANCO/825/00 rev. 6, dated 20 June 2000 [Santd et Protection des Consommateurs (SANCO)]. The evaluation of validation studies by the competent authority is conducted by comparison of these European Union (EU) requirements with the study results and most often without any practical experience of the method. Some details of this evaluation are discussed below. 

A standard format for the presentation of analytical methods is not obligatory. However, each study should contain such information normally present in complete method descriptions. The list of key points presented in the SANCO Guidance Document d may serve as a guide ... 

The Guidance Document on Residue Analytical Methods requests the applicant to assess a standard multi-residue method by using standard steps. These steps are extraction with acetone or ethyl acetate, cleanup by gel permeation chromatography (GPC) and/or silica gel chromatography and final determination by GC. 

Even if most examples and procedures presented apply to in-house validation, the procedure does not distinguish between validations conducted in a single laboratory and those carried out within inter-laboratory method performance studies. A preference for inter-laboratory studies can be concluded from the statement that laboratories should always give priority to methods which have been tested in method performance studies. Within the procedure a profound overview of different categories of analytical methods according to the available documentation and previous external validation is given. For example, if a method is externally validated in a method performance study, it should be tested for trueness and precision only. On the other hand, a full validation is recommended for those methods which are published in the scientific literature without complete presentation of essential performance characteristics (Table 9). 

If analytical methods are validated in inter-laboratory validation studies, documentation should follow the requirements of the harmonized protocol of lUPAC. " However, multi-matrix/multi-residue methods are applicable to hundreds of pesticides in dozens of commodities and have to be validated at several concentration levels. Any complete documentation of validation results is impossible in that case. Some performance characteristics, e.g., the specificity of analyte detection, an appropriate calibration range and sufficient detection sensitivity, are prerequisites for the determination of acceptable trueness and precision and their publication is less important. The LOD and LOQ depend on special instmmentation, analysts involved, time, batches of chemicals, etc., and cannot easily be reproduced. Therefore, these characteristics are less important. A practical, frequently applied alternative is the publication only of trueness (most often in terms of recovery) and precision for each analyte at each level. No consensus seems to exist as to whether these analyte-parameter sets should be documented, e.g., separately for each commodity or accumulated for all experiments done with the same analyte. In the latter case, the applicability of methods with regard to commodities can be documented in separate tables without performance characteristics. 

Guidance Document on Residue Analytical Methods SANCO/825/00 Rev. 6, Dated 20/06/00, European Commission, Brussels (2000). 

NIOSH. 1989a. NIOSH Manual of Analytical Methods. Occupational air method no. 7905. NIOSH recommendations for occupational safety and health compendium of policy documents and statements. Cincinnati, OH U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control, National Institute for Occupational Safety and Health. 

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