QC | Slide 1 of 25 June 2006 Good Practices for Quality Control Laboratories Part 3: Working procedures and safety Supplementary Training Modules on Good

QC | Slide 1 of 25 June 2006

Good Practices for Quality Control Laboratories

Part 3 :Working procedures and safety

Supplementary Training Modules on Good Manufacturing Practice

WHO Technical Report Series, No. 902, 2002. Annex 3


Incoming samples (Sampling plan and procedures)

Sample size sufficient for:– the tests to be performed– replicate tests– retained / retention sample

The laboratory must have a sampling plan and internal procedure for sampling, available to all analysts and technicians within the laboratory

Part Three. 14.1– 14.3

Quality ControlQuality Control


Test request can be filled out during sampling - accompany each sample submitted to the laboratory, and should contain the following information, e.g.:

source of the material

full description including its International Nonproprietary Name (INN), concentration or strength, manufacturer, and batch number (if available), size of the sample

reason for requesting the analysis

date on which the sample was collected

Part Three. 14.5– 14.6 (a-f)



Test request can be filled out during sampling – accompany each sample submitted to the laboratory, and should contain the following information (continued):

size of the consignment from which it was taken, when appropriate

expiry date (pharmaceutical product) retest date (starting material, pharmaceutical excipients)

pharmacopoeia specifications or other official specifications to be used for testing

record of further comments (e.g. discrepancies found)

required storage conditions Part Three. 14.6 (g-k)



Registration and labelling

All samples should be assigned a registration number

Separate registration numbers – different batches

A label with appropriate information on each container of the sample

Part Three. 14.7 – 14.8



Central register

The following information should be recorded: registration numberdate of receiptspecific unit to which the sample was forwarded

Sample received should be inspected the findings must be recorded, dated and initialled discrepancies and damage recorded queries referred back to the provider of the sample

Part Three. 14.9 – 14.10



Storage

The sample prior to testing, the retained sample and any remaining portions of the sample after performance of all required tests must be stored safely (storage conditions)

Analysis is determined by the head The sample must be stored until all relevant documentation has

been received Request for analysis may be accepted verbally only in case of

emergencies Data recorded on the analytical worksheet Copies or duplicates of all documentation must accompany each

numbered sample when sent to the specific unit

Part Three. 14.11- 14.17



Analytical worksheet

An internal document in a printed form for recording information

Complemented by the raw data obtained in the analysis

One used for each numbered sample

A further set of analytical worksheets in duplicate can be used for a collaborating unit (after testing, all results are assembled in one analytical worksheet, using the data from all collaborating units).

Part Three. 15.1 – 15.4



The analytical worksheet must provide or leave space for the following information:

registration number of the sample

page numbering including total number of pages (including annexes)

date of the test request

date of analysis performed

name and signature of analyst

description of the sample received

Part Three. 15.5



The analytical worksheet must provide or leave space for the following information (continued):

reference to the specifications to which the sample was tested including limits (adding any or special methods employed) – reference number of the specifications, if available (e.g. pharmacopoeia monograph)

results obtained of tested sample

the interpretation of the results and the final conclusions, signed by each of the analysts involved and initialled by the supervisor

the identity of the test equipment used

further comments, e.g. for internal information Part Three. 15.5 (a-k)



The above information may be complemented by:

detailed notes on the specifications selected and the methods of assessment used

whether and when portions of the sample were forwarded to other units for special tests (for example, mass spectrometry, x-ray diffraction), and the date when the results were received

identification number of any reference material

if applicable, data to be attached of an instrument verification

if applicable, data to be attached of a reagent verification

Part Three. 15.5 (i-v)



The completed analytical worksheet must be signed by the responsible analyst/s and initialled by the supervisor

Specifications necessary to assess the sample:

Particular pharmacopoeia monograph

Manufacturer’s specifications

National pharmacopoeia to be used

Specifications contained in the product licence, and should be the current version

Part Three. 15.6-15.8



Filing

Analytical worksheet filed for safe keeping together with any attachments, including calculations and tracings of instrumental analyses

If stored in a central archive – a copy should be retained in the specific unit for easy reference

Analytical test report must be prepared on the basis of the worksheet

Mistakes, amended data or text – old information may be deleted by a single line (not erased nor made illegible) and the new information added alongside, initialled or signed, and an explanation for the change given

Part Three. 15.9 – 15.12



Testing

Testing performed according to the work plan

If not feasible, the reasons noted, and the sample stored in a special locked-up place

Specific tests by a specialized external laboratory – responsible person should prepare the request and arrange for the transfer of the required number of units (bottles, vials, tablets) from the sample. Each of these units must bear the correct registration number

Part Three. 16.1. – 16.2.



Performing the tests

Official pharmacopoeia requirements – see general notices and the specific monographs of the pharmacopoeia

System suitability done as relevant

All values obtained from each test, including blank results, must immediately be entered on the worksheet, and all graphical data, whether obtained from recording instruments or hand-plotted, must be attached to the analytical worksheet

Part Three. 16.3 – 16.4.



Evaluation of test results

Results must be reviewed and evaluated – do they meet specifications?

Consider the results of all tests

Doubtful results should be investigated (internal quality system, OOS investigation, etc.)

Doubtful results can be rejected only if they are clearly due to error, which has been identified

All conclusions entered on the analytical worksheet by the analyst and initialled by the supervisor

Part Three. 17.1 – 17.2



Analytical test report:

is a compilation of the results and states the conclusion of the examination of a sample

issued by the laboratory

based on the analytical worksheet

Part Three. 17.3



Analytical test report must provide the following information:

registration numbername and address of laboratory testing the samplename and address of originator requesting analysisname and description and batch number of the sample, where

appropriate reference to the specification(s) used for testing the sample,

including limits results of all tests performed, numerical results of all tests

performed (if applicable)conclusion whether or not the sample was found to meet the

limits of specifications Part Three. 17.4



Analytical test report must provide the following information (continued):

date of test performed

signature of the head of the laboratory or authorized person

name and address of repacker/trader, if applicable

name and address of original manufacturer

compliance to requirements

date received

expiry date Part Three. 17.4



Retained samples

The purpose is to have access to the sample material for a specified period

See also basic GMP

Part Three. 18



Safety in the laboratory

– General aspects to consider. . .

Part Four.



General and specific safety instructions must be:available to each staff member andsupplemented regularly as appropriate (e.g. written material,

poster displays, audiovisual material, and occasional seminars)

General rules and SOPs should include:availability of safety data sheets to staff prior to testing being

carried outprohibition of smoking, eating, and drinking in the laboratory familiarity with the use of fire-fighting equipment, including fire

extinguishers, fire blankets, and gas masks the use of laboratory coats or other protective clothing including

eye protectionPart Four. 19.1 – 19.2



(continued)

special handling as required, e.g. for highly potent, infectious or volatile substances

full labelling of all containers of chemicals, including prominent warnings (e.g. "Poison", "Flammable", "Radiation", etc.) whenever appropriate

adequate insulation and spark-proofing of electrical wiring and equipment, including refrigerators

observation of safety rules in handling cylinders of compressed gases and familiarity with their colour identification codes

awareness of avoiding solitary work in the laboratoryprovision of first-aid materials and instruction in first-aid

techniques, emergency care, and use of antidotes Part Four. 19.2



Protective clothing must be available, including eye protection, masks and gloves

Water showers should be installed

Rubber suction bulbs used on manual pipettes and siphons

Staff must be instructed in the safe handling of glassware, corrosive reagents, and solvents, and particularly in the use of safety containers or baskets to avoid spillage from containers

Warnings, precautions and instructions must be given

Safe disposal of unwanted corrosive or dangerous products by neutralization or deactivation

Safe and complete disposal of mercury and its saltsPart Four. 19.3.



Poisonous or hazardous products

Singled out and labelled appropriately

Unnecessary contacts with reagents, especially solvents and their vapours, must be avoided

The use of known carcinogens and mutagens must be limited or totally excluded if required by local regulations

Replacement of toxic solvents and reagents by less toxic materials or reduction of their use

Part Four. 19.4


Documents

QC | Slide 1 of 25 June 2006 Good Practices for Quality Control Laboratories Part 3: Working procedures and safety Supplementary Training Modules on Good