D-111

Allergen Testing for Production Equipment

Section D — Laboratory Operations and Specifications Revision 7 9 pages

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1.0 Purpose 
 
 The purpose of this procedure is to define the use of the surface protein allergen test using
 
 3MTM Clean-Trace Surface Protein (Allergen) and Neogen Accuclean Advanced Rapid Protein
 Residue Test to demonstrate production equipment is allergen free. 
 
 2.0 Scope 
 
 This procedure describes the use of allergen test methods in the validation and refinement of
 cleaning instructions to ensure each piece of production equipment is allergen free. These
 
 allergen test methods are not valid for the testing of cleaning fluids used in removing allergen
 from production surfaces. This procedure is specific to the testing of dry production equipment
 
 surfaces. A general protein test is the primary screen for non-selective testing of protein
 
 allergens on production equipment surfaces. 
 
 3.0 Responsibility 
 
 3.1 It is the responsibility of QC Laboratory Management and/or designee to implement
 and maintain this procedure and to ensure that the procedure is being followed.
 
 3.2 ‘It is the responsibility of Quality Unit to execute monitoring activities.
 
 3.3. It is the responsibility of Production Personnel to clean production equipment as per
 
 SOP B-111 Cleaning of Manufacturing/Production Areas and Equipment and other
 
 applicable cleaning procedures. 
 
 3.4 It is the responsibility of Quality Management to review and approve all validation and
 
 test documentation and to notify production management when revalidation is required.
 
 
 

[SOP 

 Standard Operating Procedure SOP No Rev 
 Page 2 of 7 
 D-111 
 Allergen Testing for Production Equipment 
 4.0 Definitions 
 
 4.1 DC — Document Control 
 
 4.2 QC — Quality Control 
 
 4.3 AD — Analytical Development 
 
 5.0 References 
 
5.1 B-111, SOP, Cleaning of Manufacturing/Production Areas and Equipment

 3.2 C-502, SOP, Record Storage, Retention, and Destruction 
 
 5.3 D-111-F1, Form, Allergen Test Ticket 
 
 RPT-20-0007, Report, Validation of Allergen Swabs: AccuClean Advanced Rapid
5.4 Protein Residue Test

 RPT-20-0008, Report, Justification of Detection Limits for using General Protein
5.5 Swabs for Detection of Allergen Residues after Cleaning

 6.0 Equipment/Materials 
 
 6.1 Surface Protein Allergen Test Kit 
 
 6.1.1 Product 
 
 6.1.1.1 3MTM Clean-TraceTM Surface Protein (Allergen), Cat #ALLTEC60
 
 6.1.1.2 Neogen Accuclean Advanced Rapid Protein Residue Test or
 
 equivalent 
 
 6.1.2 Equipment 
 
 6.1.2.1. Biotrace International Digital Heating Block, model DHB120 or 1100.
 
 6.1.2.2 Clean-TraceTM Surface Protein (Allergen) Test Method 
 
 

[SOP 

 Standard Operating Procedure SOP No | Rev 
 Allergen Testing for Production Equipment vat! 7 Page 3 of 7 
 
 6.1.3 Specifications (3M) 
 
 6.1.3.1 Sensitivity: Screens swabs at 3u.g/100cm* surface protein
 
 6.1.3.2 Test Time: 15 minutes 
 
 6.1.3.3 Storage: Refrigerated (2°C — 8°C) 
 
 6.1.4 Specifications (Neogen) 
 
 6.1.4.1 Sensitivity: Screens swabs at 5g/100cm? surface protein
 
 6.1.4.2 Test Time: 10 seconds 
 
 6.1.4.3 Storage: Room Temperature 
 
 7.0 Procedure 
 
 Note: All employees performing allergen tests must be properly garbed (hair net, gloves, lab
 
 coat or frock, shoe covers, etc.) 
 
 7.1 All production equipment in blending, tableting, encapsulation, coating, compression,
 
 gummy, or packaging areas that has product contact with an allergen should be cleaned,
 
 swabbed, and approved before continued use. 
 
 7.1.1 After equipment is cleaned, operation personnel will notify quality that the
 
 cleaned equipment is ready to be swabbed. 
 
 7.1.2 Quality will swab NLT 5 areas from each defined equipment grouping (see
 
 attachment 1) for the presence of allergens as defined in section 7.2. Some
 equipment grouping may not contain 5 different areas for swabbing. In these
 
 cases, swabbing of each product contact area should be performed.
 
 7.1.3 Quality will prioritize hard to clean areas or any area in which accumulation of
 
 product may occur during the swabbing procedure. 
 
 

[SOP 

 Standard Operating Procedure SOP No | Rev 
 D-111 7 Page 4 of7 
 Allergen Testing for Production Equipment 
 7.1.4 Once the equipment is cleared to be allergen free, quality will notify operations
 
 that the equipment is approved for continued use. 
 
 7.2 Procedure — Surface Protein (Allergen). The instructions below are generalized for the
 3M Clean Trace and Neogen Rapid Residue test. Manufacturer’s instructions should be
 
 followed for equivalent swab technologies and more specific instructions.
 
 7 del Label a fresh Clean-Trace Surface Protein/Accuclean Advanced test tube with
 the location of the area swabbed. 
 
 Tide Remove the swab from the tube without puncturing the membrane that separates
 the liquid at the tip of the tube from the swab. 
 
7.2.3 Swab the area of approximately 10cm x 10cm (if the equipment allows) for

 Allergens. 
 
 The surface should be swabbed firmly (slight flex in the handle is acceptable)
7.2.4 with a gentle rolling motion of the swab. If applicable, Swab in one direction

 from side to side and then from top to bottom. If the surface is dry, it may be
 necessary to wet the swab with the moisturizer supplied in the kit before
 
 swabbing. 
 
 Return the swab to the tube then press down from the top until the swab head
7.2.5 penetrates the membrane and is submerged in the solution.

 7.2.6 Vortex or shake the tube from side to side for 10 seconds. 
 
 If using 3M test swabs, place the tube into the digital heating block pre-
7.2.7 equilibrated to 55°C and incubate for 15 minutes.

 7.2.8 If using the Neogen test swabs, proceed to 7.2.10 
 
 Remove the tube vertically from the digital heating block. 
7.2.9 7.2.10 Immediately note the color of the solution at the bottom of the tube.

 

[SOP 

 Standard Operating Procedure SOP No | Rev 
 D-111 7 | Page 5 of 7 
 Allergen Testing for Production Equipment 
 
 7.2.11 Document testing information and report the result on the applicable Redzone
 data sheet or on form D-111-F1 Allergen Test Ticket. 
 
 7.2.12 Report testing results to the correct personnel. 
 
 7.2.13 Due to the nature of both allergen testing swabs, any protein present will be
 
 detected as a positive reading. If multiple positive results are observed, specific
 allergen tests for the potential allergen(s) of concern in the batch ran directly
 
 before the clean may be performed to rule out that allergen’s presence.
 
 8.0 Records 
 
 8.1 Redzone is the preferred method for documentation of ATP swab results. Use form D-
 
 111-F1 Allergen Test Ticket if not using Redzone. Fill in information as follows:
 
 8.1.1 Room#- Location of equipment at the time of testing 
 
 8.1.2 Test Date — The date the test was performed 
 
 8.1.3 Description of equipment swabbed 
 
 Equipment Group — The cleaning instruction that will be impacted if the
8.1.4 cleaning validation passes or fails on any one or combination of machine tests

 (See Attachment 1). 
 
 Initial Test / Retest- Identify the iteration of test for release of equipment.
8.1.5 Test Type — indicate the specific allergen or surface protein to distinguish type

8.1.6 of allergen test being performed.

 Major Clean Performed — Identify if a major clean was performed just prior to
 
 allergen testing 
 
 Allergen Exposure — The presence or potential presence of allergens in the
8.1.8 finished product processed immediately before the major clean

 

[SOP 

 Standard Operating Procedure SOP No Rev 
 D-111 Page 6 of 7 
 Allergen Testing for Production Equipment 
 
 8.1.9 Results: The test passes if the result is negative for allergens. The result fails id
 an allergen is detected. 
 
 8.1.10 Total Result — The combined result of all swab tests. If all tests are negative, the
 survey passes. If one or more tests fail, the survey fails 
 
 8.1.11 Survey Failure — Operational Management must be notified immediately of the
 failure. The equipment must be re-cleaned and retested. 
 
 8.1.12 Repeat steps 7.2.1-7.2.12. 
 
 8.2 Allergen Test Records are maintained by the Quality Group following SOP C-502
 Record Storage, Retention, and Destruction. 
 
 9.0 Revision History 

| Rev | Date | Description of Changes | CCR # | By |
|-----|----------|------------------------|-------|----|
| 0 | 02/21/14 | New | 14-0178 | B. Johns |
| 1 | 04/21/14 | Changed from Romer EIA kits to Neogen EIA kits. Added identification of protein source. | 14-0357 | B. Johns |
| 5 | 10/06/14 | Changed from Soy 3-D Reveal EIA kit to Alert EIA kit. Added new equipment. Changelodg form. Adjusted equipment locations. Aligned SOP to present allergen | 14-0779 | B. Johns |
| 3 | 11/27/15 | test practices. Updated forms to improve clarity and traceability. Enhanced criteria for validatinga cleaning process. | 15-1142 | B. Johns |
| 4 | 10/18/17 | Added 6.1.1.4 and note for gluten in section 6.0. Updated SOP and changed title to reflect current practices and | 17-1064 | S. Millar |
| 5 | 08/19/19 | procedures. Removed Allergen validation from SOP as the current practice is to swab after every batch containianng allergen | 19-0676 | I. Garrett |
| 6 | 03/04/20 | Updated to allow the use of alternate swabs CC- = 04/18/22 Revised section 8.1 to include reference to Redzone data entry CC-22-0194 K. Burris preference. Updated logo. | 20-0172 | J. Maignan |

 10.0 Attachments 
 10.1 Attachment 1 — Major Equipment Grouping 
 
 

[SOP 

 Standard Operating Procedure SOP No | Rev om 
 Allergen Testing for Production Equipment D-111 7 Beat 
 
 Attachment 1 — Major Equipment Grouping 
 
 = = pee 3 t e é s s i e EBT E : # RPao hEe N a Gn r e RAen b e SE era ES s S SRA : Se fA . s 3 B RR B A i E S SEeR USeeeRe SSSEE S SER-38 N eaRtE S S i USE t E|t RS E : T iBoe'e ssr hRe a GGear a e rnS e}e e et e oe r n e e s B SQ& t to mR : Ei ig { —i S A O @ e e s US Ea af s | S A & R ew ; i S e q i ea P r ms e i E e t i @ ei eA t SihS e c r g e w E e r e ShcS t e E s SE t Ase e N c eeS r S s s e A i sSRe eS PEr a iSr y sEi BRC eRE v erap tePIeRrESeE EtETEhS eRyn Meeeereers3eeunr ities
 
 Blending Tableting 
 Compression Encapsulation 
 Packaging Coating 
 Gummy Liquid 
 
 

[SOP 

 IAN LABS Allergen Test Ticket 
 Form: D-111-Fl CCR No. CC-22-0194 Revision: 4 
 
 Room#: Test Date: 
 
 Equipment Group: 0 Initial Test ORetest(1 23 _ ) 
 
 Type Test (circle one): Surface Protein Other: 
 
 Previous Batch #: Formula#: 
 
 Major Clean Performed (Y/N): Allergen Exposure (Y/N): 
 
 Swab 01 
 
 Equipment Description: Result (circle one): Pass Fail 
 
 Swab 02 
 Equipment Description: Result (circle one): Pass Fail 
 
 Swab 03 LC] N/A 
 
 Equipment Description: Result (circle one): Pass Fail 
 
 Swab 04 OC N/A 
 Equipment Description: Result (circle one): Pass Fail 
 
 Swab 05 OU N/A 
 Equipment Description: Result (circle one): Pass Fail 
 
 Final Result (Circle One): Pass Fail 
 
 Test Performed By/Date: Reviewed By/Date: 
 
 
 

[SOP 

 IGNLABS Cleaning Validation Log 
 Form: D-111-F2 CCR No. CC-22-0194 
 
 Ion #: 
 Equipment Description: 
 
 Test / 
 Date Test Type __ Pass/ Fail Retest Validation Status Due Signature/Date 
 o General o Pass o Fail Initial Test o Under Validation 
 oO Milk (Cow) o Pass oFail 0 Retest 0 Validated Oo 
 o Egg (Chicken) o Pass o Fail 0 Revalidated o Next Allergen 
 0 Soy o Pass o Fail 0 Failed Validation Major 
 o General oPass oFail __o Initial Test 0 Under Validation 
 Oo Milk (Cow) oO Pass o Fail oO Retest 0 Validated o 
 0 Egg (Chicken) o Pass o Fail o Revalidated o Next Allergen 
 oO Soy o Pass o Fail 0 Failed Validation Major 
 o General oO Pass o Fail o Initial Test o Under Validation 
 o Milk (Cow) oO Pass o Fail co Retest a Validated o 
 0 Egg (Chicken) o Pass o Fail 3 Revalidated a Next Allergen 
 o Soy o Pass o Fail o Failed Validation Major 
 o General o Pass o Fail o Initial Test o Under Validation 
 0 Milk (Cow) o Pass o Fail oO Retest oO Validated oO 
 o Egg (Chicken) 6 Pass o Fail 0 Revalidated o Next Allergen 
 0 Soy o Pass o Fail 0 Failed Validation Major 
 6 General oO Pass o Fail 0 Initial Test o Under Validation 
 o Milk (Cow) o Pass o Fail oO Retest 0 Validated o 
 o Egg (Chicken) oO Pass o Fail 0 Revalidated o Next Allergen 
 oO Soy o Pass o Fail o Failed Validation Major 
 o General o Pass o Fail 0 Initial Test 6 Under Validation 
 Oo Milk (Cow) a Pass o Fail co Retest 0 Validated o 
 o Egg (Chicken) oO Pass o Fail 0 Revalidated o Next Allergen 
 Oo Soy o Pass o Fail a Failed Validation Major 
 o General o Pass o Fail o Initial Test o Under Validation 
 Oo Milk (Cow) o Pass o Fail oc Retest 0 Validated 5 
 0 Egg (Chicken) o Pass o Fail o Revalidated o Next Allergen 
 oO Soy o Pass o Fail o Failed Validation Major 
 o General o Pass o Fail o Initial Test o Under Validation 
 o Milk (Cow) o Pass o Fail oO Retest 0 Validated G 
 0 Egg (Chicken) o Pass o Fail 0 Revalidated o Next Allergen 
 oO Soy o Pass o Fail a Failed Validation Major 
 o General o Pass o Fail 0 Initial Test o Under Validation 
 a Milk (Cow) oO Pass o Fail oO Retest co Validated o 
 o Egg (Chicken) o Pass o Fail o Revalidated g Next Allergen 
 0 Soy o Pass o Fail o Failed Validation Major 
 o General o Pass o Fail o Initial Test o Under Validation 
 0 Milk (Cow) o Pass o Fail o Retest a Validated Oo 
 o Egg (Chicken) o Pass o Fail o Revalidated o Next Allergen 
 0 Soy o Pass o Fail o Failed Validation Major 
 0 General o Pass 0 Fail o Initial Test o Under Validation 
 oO Milk (Cow) oO Pass o Fail co Retest O Validated Oo 
 to Egg (Chicken) o Pass o Fail 0 Revalidated o Next Allergen 
 oO Soy o Pass o Fail a Failed Validation Major 
 o General o Pass o Fail oO Initial Test o Under Validation 
 0 Milk (Cow) o Pass o Fail oO Retest co Validated o 
 0 Egg (Chicken) o Pass o Fail 0 Revalidated a Next Allergen 
 0 Soy o Pass o Fail a Failed Validation Major 
 Second Reviewer: 
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