Analytical methods standard operating procedures

Master tiles for user, laboratory equipment, EDP devices, analytical methods, standard operation procedures, measuring schedules, sampling locations, limiting values, algorithms, customers, chemicals, literature, addresses, inventory, security instructions Planning of sampling Sample registration... 

Precision The repeatability characterizes the degree of short-term control exerted over the analytical method. Reproducibility is similar, but includes all the factors that influence the degree of control under routine and long-term conditions. A well-designed standard operating procedure permits one to repeat the sampling, sample work-up, and measurement process and repeatedly obtain very similar results. As discussed in Sections 1.1.3 and 1.1.4, the... 

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. 

Ex Analytical technique Analytical method Analytical procedure Standard operating procedure... 

Note that some organizations may not use the terminology used in this book and may not distinguish between SOPs and WIs. Standard Operating Procedures provide details of how a series of operations are carried out. An example of a SOP would be the detailed instruction for carrying out a particular analytical method. Work Instructions give details of how a specific operation is carried out. What might be classed as a WI is how to operate a particular instrument, how to estimate measurement uncertainty or how to calibrate a piece of equipment. 

FIGURE 9 Hierarchy of, relationship between, and objectives and requirements for prevalidation [106], validation [62,63, 68], and standardization of analytical methods [62, 63, 67, 68,75,84] RSD = relative standard deviation, CV = coefficient of variation, SOP = standard operating procedure. 

The following principles should be used to establish a valid analytical method A specific detailed description and protocol should be written (standard operating procedure (SOP)). Each step in the method should be investigated to determine the extent to which environmental, matrix, material, or procedural variables, from time of collection of material until the time of analysis and including the time of analysis, may affect the estimation of analy te in the matrix. A method should be validated for its intended use with an acceptable protocol. Wherever possible, tire same matrix should be used for validation purposes. The concentration range over which the analyte will be determined must be defined in the method, on the basis of actual standard samples over the range (standard curve). It is necessary to use a sufficient number of standards to adequately define the relationship between concentration and response. Determination of accuracy and precision should he made by analysis of replicate sets of analyte samples of known concentration from equivalent matrix. 

Every analytical laboratory, governmental, private, or university, has a standard set of procedures that provide both general and specific information to laboratory members. These fall into certain categories, including the laboratory s standard operating procedures (SOPs), quality assurance/quality control manuals (QA/QC manuals), procedural manuals, analytical method files, and laboratory information management systems... 

The laboratory quality control program has several components documentation of standard operating procedures for all analytical methods, periodic determination of method detection levels for the analytes, preparation of standard calibration curves and daily check of calibration standards, analysis of reagent blank, instrument performance check, determination of precision and accuracy of analysis, and preparation of control charts. Determination of precision and accuracy of analysis and method detection limits are described under separate subheadings in the following sections. The other components of the quality control plan are briefly discussed below. 

Every in vitro method should be detailed in the developer laboratories using Standard Operating Procedures (SOPs) covering all essential components and steps of the method. The SOP(s) should be sufficiently defined and described and should include the rationale for the test method, a description of the materials needed, such as specific cell types, a description of what is measured and how it is measured, a description of how data will be analyzed, acceptance and decision criteria for evaluation of data, and what are the criteria for suitable test performance. All limitations, e.g., lack of metabolic competences (presence of phase 1 and phase 2 biotransformation activities) or absence of critical transporters, should be included in the in vitro method description. In general, the in vitro method should not require equipment or material from a unique source. This may not be always possible for particular in vitro test systems or other components of the method in which case a license agreement between the provider and a recipient/user may be required. For complex and/or specialized equipment, the equipment specifications and requirements should also be described. Acceptance criteria for measurements carried out on the equipment should also be provided where applicable (e.g., for analytical endpoint determinations, linearity and limits of detection should de detailed) [2],... 

Standard operating procedures should be written by the people who will use them. They should document a procedure with sufiicient detail that another individual could recreate the procedure, but not so tightly defined that the analyst will frequently deviate from the procedure. For example, the SOP for an analytical method should specify how standards are made but should allow some leeway for the analyst to use the recipe efficiently on a day-to-day basis. The recipe to make 100 ml of a 50 mg/1 standard needs to be modified with a sentence that allows the analyst to make 50 ml or 200 ml of the standard by adjusting all volumes appropriately. 

Standard operating procedures (SOPs) are detailed descriptions of analytical methods (or of other laboratory tasks such as weighing or document archiving). 

The standard operating procedure (SOP) manual contains the procedures validated by the laboratory it is a complete set of instructions for pre-analytical, analytical and post-analytical methodology and also procedures for quality assurance/control, chain-of-custody and security. Each step in the handling of the specimen should be evaluated, optimized where possible and documented in the SOP. Important steps in the analytical process include collection, transport and accessioning of the specimen, sample preparation, isolation and detection of the analytes, production of the report and disposal of the specimen. This chapter focuses on the quality assurance and control issues for analytical method development and validation as well as statistical representation of the data. 

Each separate test facility unit or area should have immediately available current Standard Operating Procedures relevant to the activities being performed therein. Published text books, analytical methods, articles and manuals may be used as supplements to these Standard Operating Procedures. 

In the case of compxrsitional data, a lot of analytical techniques can be chosen. Analytical procedures based on these techniques are then selected to be aprplied to the samples. Selected analytical methods have to be fully validated and with an estimation of their uncertainty (Gonzalez Herrador, 2007) and carried out in Quality Assurance conditions (equipment within sp>ecifications, qualified staff, and documentation written as Standard Operational Procedures...). Measurements should be carried out at least duplicate and according to a given experimental design to ensure randomization and avoid systematic trends. 

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