Chemistry Checklist for the Technical Assessment of Agriculture and Food Products Testing

CHEMISTRY CHECKLIST FOR THE TECHNICAL ASSESSMENT OF AGRICULTURE AND FOOD PRODUCTS TESTING LABORATORIES

CAN-P-1588 October 1998

PROGRAM SPECIALITY AREA – AGRICULTURE AND FOOD PRODUCT TESTING LABORATORIES [PSA-AFP]

The Standards Council of Canada 45 O’Connor Street, Suite 1200 Ottawa, Ontario K1P 6N7 Canada About the Standards Council of Canada

The Standards Council of Canada ("Council") is a crown corporation established by an Act of Parliament in 1970 to foster and promote voluntary standardization in Canada. It is independent of government in its policies and operations, although it is financed partially by Parliamentary appropriation. The Council consists of members from the government and private sectors.

The mandate of the Council is to promote the participation of Canadians in voluntary standards activities, promote public-private sector cooperation in relation to voluntary standardization in Canada, coordinate and oversee the efforts of the persons and organizations involved in the National Standards System, foster quality, performance and technological innovation in Canadian goods and services through standards-related activities, and develop standards-related strategies and long-term objectives.

In essence, the Council promotes efficient and effective voluntary standardization in Canada in order to advance the national economy, support sustainable development, benefit the health, safety and welfare of workers and the public, assist and protect consumers, facilitate domestic and international trade and further international cooperation in relation to standardization.

In addition, the Council serves as the government's focal point for voluntary standardization, represents Canada in international standardization activities, sets out policies and procedures for the development of National Standards of Canada, and for the accreditation of standards development organizations, of certification organizations, of calibration and testing laboratories, of quality management systems registration organizations, and of environmental management systems registration organizations, and promotes and supports the principle of recognition of accreditation or equivalent systems as a means of decreasing the number of multiple assessments and audits, both in Canada and with Canada's trading partners.

This document is one of several issued by the Standards Council of Canada to define the policies, plans, and procedures established by the Council to help achieve its mandate.

Requests for clarification and recommendations for amendment of this document, or requests for additional copies, should be addressed to the publisher.

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The Standards Council of Canada

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October 1998 Page 2 of 21 PREFACE

The Standards Council of Canada (SCC) has established a working group to determine specific requirements for laboratories involved in microbiological and/or chemical testing of food, feed and fertilizer. Representation currently includes the private laboratory sector, federal and provincial governments.

The role of the working group is to:  amplify the requirements necessary for laboratories working in these disciplines and areas  use existing international and national documents wherever possible

The key technical areas identified were:  interpretation of ISO/IEC Guide 25  proficiency testing  technical assessors checklist (CAN-P-1588 and CAN-P-1589)

This voluntary accreditation program is intended for laboratories that perform testing of food, feed, and fertilizer for:  chemical analysis ranging from percent levels to trace levels  qualitative and quantitative microbiological analysis.

The goal is to establish a minimum standard for quality and a uniform level of proficiency. This document identifies the minimum requirements for accreditation of laboratories supplying food and agricultural input testing services.

Accreditation under this program is the formal recognition by the Standards Council of Canada of the competence of a food, feed and fertilizer testing laboratory to perform and control chemical and microbiological testing. (ANNEX I of CAN-P-1587 contains definitions for food, feed and fertilizer)

Accreditation is not a guarantee of correct test results nor is it replacing contractual requirements between a laboratory and its client.

of 21 October 1988 1.0 Introduction.

This checklist is intended to provide specific questions and guidance to technical assessors conducting laboratory on-site assessment and reassessment under the PSA-AFP of the SCC Program for Accreditation of Laboratories. The checklist is designed to assist the technical assessor in determining whether or not a laboratory is technically competent to carry out chemical tests of agriculture and food products. The guide is a technical supplement which should be used in conjunction with the SCC application/checklist form, CAN-P-1510C, Guidelines for Preparing an Application for Accreditation for Calibration and Testing Laboratories and any specific assessors checklist for each assessment or reassessment assignment.

It is essential that the test methodology and the quality system manual be reviewed prior to an audit and as a result from this review a specific checklist may be prepared. Points raised here are to be considered when developing the checklist but are not all inclusive.

Space for comments has been provided at the end of each section. Conformity to the recommended procedures is noted by the following coding system: S: Satisfactory, Ni: Needs improvement, Un: Unacceptable, M: Missing and Na: Not applicable in the provided check box.

2.0 Definitions

For the purposes of this document, the relevant definitions given in ISO/IEC Guide 2, 30 and VIM, and the terms and definitions of CAN-P-1587 apply.

NOTE ISO 8402 sets out the general definitions related to quality whereas ISO/IEC Guide 2 sets out the definitions specifically related to standardization, certification and laboratory accreditation. Where different definitions are given in these publications, the definitions in ISO/IEC Guide 2, 30 and VIM are preferred.

3.0 References:

For the purposes of this document, the references given in CAN-P-1587 apply.

October 1998 Page 4 of 21 4.0 Accreditation Requirements

4.1 General Requirements

Laboratories must meet all the pertinent provisions of:  CAN-P-4C : 1991, General Requirements for the Accreditation of Calibration and Testing Laboratories,  CAN-P-1515 : 1991 Conditions for the Accreditation of Calibration and Testing Laboratories.  CAN-P-1587 : 1998, Guidelines for the Accreditation of Agriculture and Food Products Testing Laboratories

For details on preparing an application see:

 CAN-P-1510 : 1992, Guidelines for Preparing an Application for Accreditation for Calibration and Testing Laboratories

4.2 Chemistry Testing Requirements

In addition, laboratories performing chemical analysis must also meet all the requirements of CITAC Guide 1 “International Guide to Quality in Analytical Chemistry, an aid to Accreditation”. December 1995, 1st edition

4.3 Microbiology Testing Requirements

In addition, laboratories performing microbiological analysis must meet the requirements of “Eurochem/EAL Accreditation for Laboratories Performing Microbiological Testing” April 1996 (See ANNEX 2 of CAN-P-1587 for specific interpretations).

of 21 October 1988 Laboratory : Technical Assessor : SCC 1003-15/

Items to Verify Code Comments 5. Personnel 5.1 Are there established criteria for staff: knowledge and skills; accountability and any other related information for each level of responsibilities?

5.2(a) Are there current (<3 years old) detailed job specifications for each staff position? (b) Do they include detailed QC responsibilities?

5.3 Are individual qualifications on file and updated regularly?

5.4 Is there a performance review program?

5.5 Is there an established and relevant staff training and development program?

5.6 Is there formal documentation of progress during training?

5.7 Is there documented evidence of continued analyst proficiency for each test/method performed? Frequency

5.8 Are there backup personnel identified for critical positions?

5.9 (a) Does the laboratory provide in-house training on quality?

(b) Is it a continuing program? (c) What type? Describe.

SIGNATURE S: Satisfactory Ni: Needs improvement Un: Unacceptable M: Missing Na: Not applicable

October 1998 Page 6 of 21 Laboratory : Technical Assessor : SCC 1003-15/

Items to Verify Code Comments Comments:

6. Equipment

6.1 All instruments required for the test procedure are available and functioning properly (See Appendix 1).

6.2 All support equipment required for the test procedure is available and functioning properly (See Appendix 1).

6.3 Periodic performance checks carried out and documented.

6.4 Record of calibration and maintenance available.

6.5 Can calibrations be traced to national or international standards?

6.6 Equipment situated in an appropriate environment.

Comments:

6.7 Out of service equipment identified and not in use.

6.8 Is there documented evidence of validation for new equipment and for repaired equipment found out of service before reuse? 6.9 Are up to date equipment operating instructions available?

Items to Verify Code Comments 6.10 Is there a formal procedure to revalidate the equipment not regularly used?

6.11 Use of Computers:

(a) Is evidence of validation of software used for the purpose of communication of analytical work available?

(b) Is complete documentation for validation purposes available for in-house software?

(c) If the laboratory operates a computerized data/information management system (LIMS), are there backup systems to ensure integrity and availability of data/information in the event of a system/power failure?

(d) Are computer software program and test data backup copies secured?

(e) Are there procedures in place to prevent corruption of the system (e.g. Virus scans)?

(f ) Is accessibility to the computer system controlled? Comments :

7. Reagents, Reference Materials and Supplies

7.1 Reference materials identified and traceable to primary standards or national or international sources.

Items to Verify Code Comments 7.2 Comparison or verification of reference material before use.

7.3 Documentation and protocol when nonconforming results are encountered.

7.4 All reagents, reference materials, and supplies required for the test procedure are available and meet the specifications outlined in the method.

7.5 Reagents, reference materials and supplies are stored under the appropriate /recommended conditions.

7.6 Reagents and reference materials are stored under conditions which insure the separation of incompatible materials and in a secure manner.

7.7 Are analytical reagents properly labelled with material, concentration, solvent , date of preparation, expiration date, identity of person preparing, reference to analysts logbook?

7.8 Reference solutions prepared and diluted using specified volumetric glassware and calibrated pipettes.

7.9 Is glassware properly cleaned and rinsed?

7.10 Where the quality of a reagent is critical to a test, the quality of a new batch is verified against the outgoing batch provided that the outgoing batch is still serviceable. Other means could be used, such as testing of reagents

7.11 Are reagents disposed of in a proper manner?

Comments :

Items to Verify Code Comments

8. Test Method

8.1 Method specified in the SCC scope is being used. List test methods checked at the time of the assessments or reassessment.

8.2 Latest approved version of the test method are assessable and being used.

8.3 Any change to the test method is documented and validated.

8.4 Method Contains:

(a) ) Scope and field of application

(b) References

(c) Principles and Definitions

(d) Reagents and Materials

(e) Apparatus

(f) Sub-sampling (test sample, test portion)

(g) Analytical methodology

(h) Expression of Results

(i) Representative documents (e.g. chromatograms, other data output)

(j) Performance criteria

(k) Critical control points (temperature, lighting, brown glass, etc)

(l) Method of identifying the most recent approved test method (version number, etc)

(m) Revision history

(n) Safety

Comments :

8.5 Validation of Method:

(a) Specificity of the method in a given matrix

(b) Range

(c) Linearity

(d) Limit of Detection

(e) Reporting Limit

(f) Accuracy

(g) Precision

(h) Confirmation techniques

(i) Repeatability

(j) Validation of test method performed under same conditions as those of a real assay (Matrix etc.)

(k) Criteria for required valid number of SIGNATURE S: Satisfactory Ni: Needs improvement Un: Unacceptable M: Missing Na: Not applicable

Items to Verify Code Comments samples tested

(l) Availability of validation data

(m) Verification of method modifications

(n) Measurement of uncertainty

Comments :

8.6 Quality Control:

(a) Frequency and number of standards per sample batch

(b) Duplicates (Precision)

(c) Reference samples

(d) Analytical spikes

(e) Method blanks

(f) Critical control points

(g) Intralaboratory check samples are run with each series of samples along with blanks, internal standards, etc.

(h) How are out of control situations identified (i.e. nonconformance criteria)?

(i) Is there a formal corrective action process for out of control situations?

(j) Control charting

Items to Verify Code Comments (k) Corrective actions taken

Comments:

8.7 Interlaboratory Check Samples

Note : As per CAN-P-1587, the laboratory must participate in specified PT programs. Please review their data records for each program. Other PT programs not specified by CFIA or SCC should be reviewed as well.

(a) List current proficiency testing programs in which the Laboratory participates and their frequency. (additional information may be attached as required)

Program, Names/Matrix/Test, Frequency

(b) Are there feedback and corrective action programs, procedures and protocols for the proficiency testing programs.

9. Test Conduct

9.1 Sample Handling :

(a) Established acceptance/rejection criteria for laboratory samples

Items to Verify Code Comments (b) Does a sample control system exist within the laboratory?

(c) Procedure for the selection of test portions (subsamples0

(d) Is the laboratory sample stored under conditions to protect the integrity of the sample?

(e) Documentation of procedures followed when not specified in the method.

(h) Procedure for ensuring no cross contamination during subsampling.

(i) Labels unambiguously identify the laboratory sample.

(j) Is there a sample disposal procedure? Is there evidence that the laboratory policies and practices are in place and are in compliance with regulatory requirements?

Comments:

9.2 Method followed :

(a) Preparation steps are followed.

(b) Standards/reagents criteria for storage and use met.

(c) Standards are allowed to come to room temperature before use.

(d) All QA/QC samples run

Items to Verify Code Comments (e) Steps in the written procedure are followed.

Comments :

9.3 Supporting documents followed :

(a) Equipment instruction manuals or operating procedures .

(b) Software procedures

(c) Glassware procedures.

(d) Supporting test methods.

(e) Reporting procedures.

Comments :

9.4 Analysts records

(a) Test data including QC

(b) Calibration data

(c) Analyst ID, extraction procedures

(d) Sample ID

(e) Equipment ID

(f) Test method ID

(g) Date of Test

Items to Verify Code Comments (h) Verification checklist

Comments :

10. Measurement Traceability

10.1 Procedure to ensure traceability to national or international measurements standards where available.

Note : evidence shall be through certificates from national standards laboratories or a laboratory accredited for calibration. If these routes are not available, tracebility shall be provided by a body recognised by the accreditation organization for the measurement concerned.

10.2 Where traceability to national standards is not possible or relevant what other means are used to provide confidence in the results?

(a) Interlaboratory comparisons

(b) Proficiency testing

(c) other ( e.g. testing by an alternative method)

10.3 Where applicable, the following should be checked :

(a) Are thermometers/thermocouples used for checking temperatures of incubators, refrigerators and freezers certified and/or calibrated against a reference thermometer (traceable to a national standard0?

Items to Verify Code Comments Frequency of calibration checks : Documentation of calibrations, certificates available:

(b) Check/calibration weights : Traceable to national or international standards? Sent for recalibration at scheduled intervals? Frequency:

(c) Ovens : Temperatures checked and recorded? Frequency (minimum once daily)? Oven maintenance and repair record available? Instruction manual available?

(d) Refrigerators : Temperatures checked and recorded? Frequency (minimum once daily)? Interior/exterior cleaning schedule available? Defrosting (documented frequency)?

(e) Water baths : Temperatures checked and recorded? Frequency (minimum prior to use)? Baths cleaned our regularly (documented frequency)? Bactericide used?

(f) Balances : Balances cleaned after each use? Monthly verification checks with standard weights? Class of standard weights? Certificate of traceability Calibration date?

(g) pH meter: PH standards available pH 4.0, 7.0 et 10.0? SIGNATURE S: Satisfactory Ni: Needs improvement Un: Unacceptable M: Missing Na: Not applicable

Items to Verify Code Comments Probes maintained with cap on and/or in buffer solution or distilled water according to manufacturers instructions? Manual/Manufacturer’s instructions available?

(h) Pipettors : Initial verification of volume delivered checked? Regular checks to ensure that the equipment is performing within the required specifications? Calibration checks (frequency may depend on usage)?

(i) Hygrometers – where humidity is important to the outcome of the test Calibration to national/international standards?

(j) Timers : Verified using a calibrated timer or the national time signal?

(k) Glassware : Is borosilicate glassware used? Is all glassware cleaned in a manner consistent with testing protocols/methods being applied? Is the accuracy of volumetric glassware ensured through calibration checks or use of Class A glassware? Is Class A volumetric glassware dried by heating. Method used :

Items to Verify Code Comments An example of a method is to use a solution of 0.1g Bromthymol Blue in 8ml of 0.02N NaOH and make up to 250ml with distilled water. The reactions are pH less than 6.5 = yellow, pH between 6.5 and 7.3=blue-green, pH greater than 7.3 =blue. Check several pieces of glassware. Comments :

11. Data Management :

11.1 Instrument records :

(a) ID and operating conditions

(b) All calculations used to generate data

(c) Final chromatograms/spectra

(d) Verification of data transfer and calculations

(e) Limited access to unauthorised change of raw data

Comments :

11.2 Analyst record keeping:

(a) Permanent records of weights, analysis values, sequences, observations and calculations. (e.g. lab books, numbered sheets)

(i) Name, unit, date of entries

(ii) Table of contents

(iii) Pages numbered sequentially and completed

(iv) Entries in ink

(v) Corrections : single strikeout line, initialled, dated and explained.

(vi) Method included or referenced.

(vii) Method deviations noted and initialled by supervisor..

(viii) Unique ID for samples, standards and reagents.

(ix) All primary data (quantities, weights, dilutions, volumes).

(b) Procedures for changes to permanent records.

(c) Ensure that the final reported result is the same as reported by analyst.

Comments :

An example of a checklist prepared to ensure that proper calibration and performance verification procedures have been carried out for a Gas Chromatograph/Mass Spectrophotometer. Similar lists can be prepared by the technical assessors for other pieces of equipment.

Gas Chromatography / Mass Spectrometry Checklist

1) Does the lab have a written procedure for the set-up and Yes No Documented operation of the GC/MS instrument? 2) Are septa changed at specified intervals? 3) Are liners changed cleaned / replaced at specified intervals? 4) Does your laboratory have written criteria for corrective action of unacceptable instrument performance? 5) Is the performance of a new column evaluated before use? 6) Does the IS have similar chemical and physical properties to that of the analyte? 7) If your lab uses historical calibration for an assay, are calibrators and or/controls run with each batch of specimens- for analysis for check stability of the calibration? 8) Does your lab check for carry-over? 9) Does your lab determine the linearity of each assay periodically? 10) Does your lab determine the detection limit for each assay periodically? 11) Does your lab have written criteria for an acceptable mass spectrometer tune? 12) If the tune is unacceptable, is corrective action taken? 13) Does your lab maintain records of mass spectrometric tuning?

14) If your lab uses selected ion monitoring for identification, does it compare ion ratios and retention times between calibrators, controls and specimens? 15) If your lab uses full scan mass spectral identification through library searching, are there documented criteria for acceptability? 16) Does your lab maintain written documentation of training of personnel in the following (where applicable) ?: a) extraction procedures b) theory of operation and software c) full scan mass spectral identification d) selected ion monitoring e) quantitation

of 21 October 1988