Presentation on theme: "A planned set of activities necessary to provide adequate confidence that requirements are properly established and products or service conform to specified."— Presentation transcript:
A planned set of activities necessary to provide adequate confidence that requirements are properly established and products or service conform to specified requirements. Sets up measurement programs to evaluate processes. Identifies weakness in process and improves them. The process by which product quality is compared with applicable standards; and the action taken when nonconformance detected. An activity which verifies that the process meets pre-defined standards.
To document the procedures and methods of sample collection, preparation and analysis. To provide assurance as to reliability of analyses using replicate samples, cross-laboratory checks and an “known reference” standards. To provide assurance as to the precision from duplicate samples. To provide assurance as to the accuracy from using recognized reference standards. To provide reliable information regarding the interpretation of the data. To provide a chain of custody of samples. Bruce W. Downing, M.Sc., P.GeoBruce W. Downing, M.Sc., P.Geo. is Senior Geologist, Gamah International Ltd., Vancouver.
21 CFR PART 58 - Food and Drug Administration 40 CFR PART 160 – Environmental Protection Agency http://www.accessdata.fda.gov/scripts/cdrh/cfdocs/cfcfr/CFRSearch.cfm?CFRPart=58 http://ecfr.gpoaccess.gov/cgi/t/text/text-idx?c=ecfr&sid=68585f39e9accd101eb9a716f01fc95e&rgn=div5&view=text&node=40:18.104.22.168.11&idno=40
(a) Must designate a study director. (b) Must have a quality assurance unit. “A testing facility shall permit an authorized employee of the Food and Drug Administration to inspect the facility and to inspect all records and specimens required to be maintained regarding the study.”
Each testing facility shall be of suitable size and construction and shall be designed so that there is a degree of separation that will prevent any function or activity from having an adverse effect on the study. As necessary to prevent contamination or mixups, there shall be separate areas for: (1) Receipt and storage of the test and control articles. (2) Mixing of the test and control articles with a carrier, e.g., feed. (3) Storage of the test and control article mixtures. Space shall be provided for archives, limited to access by authorized personnel only, for the storage and retrieval of all raw data and specimens from completed studies.
(a) Each individual shall have education, training, and experience, or combination thereof, to enable that individual to perform the assigned functions. (b) Each testing facility shall maintain a current summary of training and experience and job description for each individual engaged in or supervising the conduct of the laboratory study.
A scientist or other professional of appropriate education, training, and experience, shall be identified as the study director. The study director has overall responsibility for the technical conduct of the study, and represents the single point of study control. (a) Approves the protocol, including any changes. (b) All data, including observations of unanticipated responses are accurately recorded and verified. (c) Unforeseen circumstances that may affect the quality and integrity of the study are noted when they occur, and corrective action is taken and documented. (e) All good laboratory practice regulations are followed. (f) All raw data, documentation, protocols, specimens, and final reports are transferred to the archives during or at the close of the study.
(1) A descriptive title and statement of the purpose of the study. (2) Identification of the test and control articles. (3) The procedure for identification of the test system. (6) A description of the experimental design, including the methods for the control of bias. (4) A description and/or identification of solvents, emulsifiers, and/or other materials used to solubilize or suspend the test or control articles before mixing with the carrier. (5) The type and frequency of tests, analyses, and measurements to be made. (6) The records to be maintained. (7) A statement of the proposed statistical methods to be used.
A testing facility shall have a quality assurance unit which shall be responsible for monitoring each study to assure management that the facilities, equipment, personnel, methods, practices, records, and controls are in conformance with regulations. For any given study, the quality assurance unit shall be entirely separate from and independent of the personnel engaged in the direction and conduct of that study.
(1) Maintain a copy of a master schedule sheet containing the test system, nature of study, date study was initiated, current status of each study. (2) Maintain copies of all protocols pertaining to all laboratory studies for which the unit is responsible. (3) Inspect each laboratory study and maintain written and properly signed records of each periodic inspection. Any problems found during the course of an inspection which are likely to affect study integrity shall be brought to the attention of the study director and management immediately. (5) Determine that no deviations from standard operating procedures were made without proper authorization and documentation. (6) Review the final study report and assure that the reported results accurately reflect the raw data of the laboratory study.
Equipment shall be adequately inspected, cleaned, and maintained, and shall be adequately tested, calibrated and/or standardized according to the Standard Operating Procedures, and the person responsible for the performance of each operation shall be designated. Shall specify action to be taken in the event of failure or malfunction of equipment. Written records shall be maintained of all inspection, maintenance, testing, calibrating and/or standardizing operations.
A testing facility shall have standard operating procedures in writing setting forth study methods that insure the quality and integrity of the data generated in the course of a study. All deviations in a study from standard operating procedures shall be authorized by the study director and shall be documented in the raw data. Significant changes in established standard operating procedures shall be properly authorized in writing by management.
(a)The identity, strength, purity, etc. which will appropriately define the test or control article shall be determined. (b) The stability of each test or control article shall be determined. (c) Each storage container shall be labeled by name or code number, batch number, expiration date-if any. (d)Each container shall also be labeled with appropriate, storage conditions necessary to maintain the identity, strength, purity, and composition of the test or control article. (e) There is proper storage. (f) Distribution is made in a manner designed to preclude the possibility of contamination, deterioration, or damage. (g) Proper identification is maintained throughout the distribution process. (h) The receipt and distribution of each batch is documented with the date and quantity of each batch distributed or returned.
Chain of Custody An acceptable QA/QC program will require that the complete history of every sample taken for evaluation be recorded. Such a history will include: 1. The date, time and sampling protocol for the original sample. 2. The method, duration and location of any sample storage. 3. A detailed record of any physical or chemical treatment of the sample, including drying, crushing, grinding, screening, splitting, and washing. 4. A record of all personnel who have handled the sample, including time and place. 5. Records of all disposals of sample parts, fractions and splits. This "cradle to grave" record allows an investigator to follow the chain of custody backwards in order to investigate unusual or unexpected results.
University of California DANR Analytical Lab Quality Control for Laboratory Analyses: BLANKS – A reagent blank is analyzed with every set of samples that are extracted or digested. This reagent blank includes any and all reagents that are used in the analytical process and is carried through the entire process, including extraction and filtering or digestion. DUPLICATES – At least ten percent of samples are analyzed in duplicate. The first, last and every tenth sample are run in duplicate. Duplicate values typically should fall within 8% of each other for all samples unless sample homogeneity is a problem. This information is included in the report.
University of California DANR Analytical Lab STANDARD REFERENCE MATERIALS – At least one standard reference material is analyzed with each set of samples. The values for the standard reference materials are included in the final report. Samples run with a standard reference material that falls outside the acceptable range are reanalyzed, including digestion or extraction if necessary. SPIKE SAMPLES – Sample fortifications or spikes are used to verify accuracy of tests requiring extensive sample manipulation (such as acid digestion) or for non-standard sample types. SAMPLE EXCHANGE AND CERTIFICATION PROGRAMS - The ANR Analytical Laboratory participates in a number of sample exchange and certification programs. The Laboratory participates in the International Plant Exchange for plant material and the North American Proficiency Testing Program for soils, water and plant material and manure.
Virginia Institute of Marine Science The following Quality Control Criteria are the basic parameters monitored by the analyst at the bench. An Investigator may specify absolute limits or additional protocols as required for the project. Correlation - Calibration curve coefficient must exceed 0.999. Standard Reference Materials - Analyzed daily, matrix matched, mid-range concentration, must meet statistical control limit (internal) for lot. Intercept Correction - Employed to eliminate any standard matrix artifacts not applicable to samples.
Virginia Institute of Marine Science Precision - 10% Duplication - Randomly chosen, not linked to field duplication. Control limits derived from past data in similar concentration range and matrix, or specified by investigator. Accuracy - 10% Spiking - Recovery of known addition added directly to sample to verify the control of matrix interferences. Statistical control limited. Failure to meet criteria triggers interference screening and method modification. Baseline correction - Zero analyte response verified every 10 samples. Drift mathematically compensated. Sensitivity Correction - Calibration verified every 10 samples. 10% deviation triggers re-calibration. Drift below 10% mathematically corrected.
There shall be archives for orderly storage and expedient retrieval of all raw data, documentation, protocols, specimens, and interim and final reports. Depending on the study or funding agency these records must be retained for from 2-5 years.