Professional Documents
Culture Documents
PRESENTED BY JEAN COBB SENIOR PROJECT ASSOCIATE PESTICIDE RESIDUE LAB For Field and Laboratory Research BIOCHEMISTRY
ALS 5204
Key Dates
1970 1980
1976 FDA GLP proposed
1990 2000
One of the first names to attract regulatory and media attention was IBT
Industrial Bio-Test Laboratories (IBT), Craven BioLabs, Intertek Testing Services, & others
Submits Regulatory Data Yes! Permission to Market Regulated Product
Sponsor
Approve?
Test Facility: Field and laboratory (contract) research facilities Sponsor: Pharmaceutical and pesticide manufacturers
Sponsor
Approve?
Would you want the FDA to issue a permit to manufacture of a drug based on sloppy research? Or for the EPA to register a pesticide based on fraudulent data? Probably not!
Approve?
External audits and inspections of sponsor and test facility (conducted by regulatory agency)
GLP Regulations
Documentation (Tools)
Training records, CVs, GLP training Maintain adequate space/separation of chemicals from office areas Calibration, logbooks of use, repair, and maintenance; check freezers Standard operating procedures Chemical and sample inventory, track expiration dates, labeling Timely reporting, storage of raw data and reports
Documentation
If you didnt write it down, it NEVER happened. (As far as an auditor is concerned)
Auditor/ Inspector
Equipment
40 CFR Part 160 (EPA GLP regulations)
Section 160.63 Maintenance and Calibration 160. of Equipment. (a) Equipment used in the generation, measurement, or assessment of data shall be adequately tested, calibrated, and/or standardized. (c) Written records shall be maintained of all inspection, maintenance, testing, calibrating, and/or standardizing operations. Do you know the difference between standardized, calibrated, and verified?
Equipment
Verification (Testing): external check of equipment accuracy (check balance accuracy against weights at laboratory- no adjustment) laboratory Calibration: equipment is adjusted based on comparison to certified or known reference materials (balance adjusted after comparison to certified weights by trained professional) Standardization: comparison with similar equipment (use two thermometers of similar design to compare readings)
Equipment
What about validation?
Electronic data management systems (computers, instrumentation) must be validated to confirm that they will perform their intended functions For example, a computer spreadsheet used for calculations during a GLP study could be validated as follows: enter identical raw data as previously and compare the calculations using the same software/options- they should software/optionsbe identical!
Use Logbooks
AGILENT GAS CHROMATOGRAPH SERIES: 6890n VT#0000322580
DATE 9/13/07 NAME John Smith (lab tech)
PROJECT SAMPLE MATRIX DETECTO R TYPE COLUMN TYPE/ SIZE OVEN TEMP c INLET TEMP c DET TEMP c GAS mL/min ROUTINE SERVICE (#) PROBLEM (#)
VCE07020
Water
60-275C
250C
350C
N/A
9/14/07
VCE07021
Plant Tissue
90-275C
250C
350C
N/A
9/17/07
Standards only
N/A
NPD
60-275C
225C
300C
N/A
Record all pertinent operating parameters Take the time to record routine service and how problems were resolved (it may help if/when the same problem arises!)
Equipment
Was the equipment functioning properly? Who performed the work, what was the date, and what specific parameters did they use? What was there a problem? How was the problem fixed?
Question: Which takes precedence: the manufacturers expiration date or expiration date as stated in the facility SOPs? Answer: Whichever is earliest!
Use Labels
Clearly label chemicals and solution containers Make sure that the expiration date and storage requirements are included on the label If a solution, what date was it prepared?
CHEMICAL LABEL CHEMICAL___ ____________ ________ CHEM ID#______________________________ _ DATE RECEIVED:___________________________ DATE OPENED: ____________________________ EXPIRATION DATE__ _ _______STORAGE______
SOLUTION LABEL CONCENTRATION_____________________ SOLUTION____________________________ FROM CHEM ID#_____________________ DATE PREPARED_____________________ EXPIRATION DATE______ STORAGE______
Use Forms
PESTICIDE RESIDUE LABORATORY 2007 CHEMICAL INVENTORY FORM LAB CHEMICAL ID (s): __C070014______________
Assign a unique number to each chemical received by the facility Record the purity, date received, storage conditions, and source Use the form to jog your memory about the information you need to collect
CHEMICAL NAME: ethyl acetate CAS NO.: 141-78-6 SOURCE: Fisher Scientific LOT NO.: 067720 PURITY/GRADE: Pesticide Grade QUANTITY RECEIVED: 4 L EXPIRATION DATE: 9/7/12 STORAGE CONDITIONS: ambient, in solvent cabinet DATE RECEIVED: 9/7/07 SIGNATURE:
Jean M. Cobb
COMMENTS: N/A
Raw Data
Question: What happens if you make a mistake?
Answer: Do not obscure original data!! Instead, draw a single strikeout, then add reason code, initials, and date of change. (Preserve the original data).
Documentation
Record data using permanent ink (never pencil) Date and sign every entry (who is responsible?) Keep records in real time (no catching up later) No rewrites, need original entries (reduces rewrites, transcription errors)
Raw Data
40 CFR Part 160 (EPA GLP regulations) Section 160.3 Definitions. Raw data 160. Raw means any laboratory worksheets, records, memoranda, notes, or exact copies thereof, that are the result of original observations and activities of a study and are necessary for the reconstruction and evaluation of the report of that study.
If you scribble some notes on a scrap of paper, are those notes considered raw data? Answer: Yes!
Raw Data
Can you list examples of raw data?
Logbooks (to record temperatures or equipment use, repair, and maintenance) Field or laboratory notebooks Forms (for field or laboratory observations, chain-ofchain-ofcustody, sample or chemical receipt) Training reports Computer printouts Recorded data from automated instruments
Answer: You dont have to thats one of the functions of the Standard Operating Procedures (SOPs).
Writing Guidelines
Cautions:
Avoid restrictive language such as vortex for exactly 1 minute but include clear instructions such as vortex until homogenized if that satisfies the purpose Dont add unnecessary steps such as consult the manual unless personnel are required to follow this step
Writing Guidelines
The primary goal is to avoid confusion
Did your supervisor say to make a 1 in 4 dilution or was it a 1 to 4 dilution? If it is written in an SOP, the instructions can be verified.
GLP Compliance
Not Required: Basic research (most of the research conducted at universities like Virginia Tech) Studies to develop new analytical methods Chemical tests used to derive the specifications of a marketed food product Instead, emphasize GLP principles during research
GLP Principles
GLP principles are a good idea even if you are not required to comply with the regulations.
Say What You Do (with written standard operating procedures) Do What You Say (follow the procedures) Be Able to Prove It (with good record keeping)
GLP Experience
An employer may find it useful if you have: Practical experience with working on a study conducted in compliance with GLP regulations Experience working at a facility that emphasizes GLP principles Familiarity writing and using standard operating procedures at a GLP facility
Fulfil the legal requirements of some FDA and EPA research studies
Websites
Code of Federal Regulations (CFR)- all (CFR) EPA GLP Regulations FDA GLP Regulations USDA- Pesticide Data Program (PDP) USDAStandard Operating Procedures