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Standard Operating Procedure (SOP) for Contract Laboratory Agreement and analytical testing. It covers all the processes of sample sending, sample analysis, and report review of the contract testing laboratory.

Contract Laboratory Agreement and Testing

1.0   PURPOSE:

• • To provide guidance to audit and approval of contract analytical testing laboratory as per cGMP requirement.
  • To provide guidance for sample sending, sample analysis, and report review of contract testing laboratory.

2.0   SCOPE:

• • This procedure is applicable to the analysis performed at outside contract laboratories or inter-location laboratories.

3.0   REFERENCES:

• • FDA Guidance on Quality Matrics

• • In House

4.0   RESPONSIBILITY – SOP FOR CONTRACT LABORATORY:

• •  Analyst shall be responsible for :

• •  To send the sample for testing and review the report of contract laboratories as per the SOP.

• •  Packing of the sample and prepare the test request slip.

• •  To provide the reference ATP, reagents, impurities/WS to contract laboratory as  and when required.

• • Quality Control Head or Designee shall be responsible for:

• • Review of the SOP

• • Ensure implementation and adherence to the system as per the SOP.

• • Provide the training to the concerned persons before the implementation of the SOP.

• • Audit the contract laboratories as per the SOP as and when required.

• • Review the contract testing laboratory audit report and ensure the compliance of the audit query.

• • Prepare Quality Agreement Documents.

• •  Quality Assurance shall be responsible for :

• •  To check the SOP

• •  To ensure the implementation of the system as per the SOP.

• •  Quality Assurance Head or Designee shall be responsible for :

• •  Approval of the SOP.

• •  Ensure the implementation of the system as per the SOP.

• •  Review the contract testing laboratory audit report and ensure the compliance of the audit query.

• •  Approve the contract testing laboratory for testing of samples.

• •  Approve quality agreement documents.

5.0   ABBREVIATION:

• • AR.No. : Analytical Report Number

• • ATP: Analytical Test Procedure

• • B.No. : Batch Number

• • cGMP: Current Good Laboratory Practices

• • COA: Certificate of Analysis

• • FDA: Food and drugs Administration

• • LIMS: Laboratory Information Management System

• • OOS: Out of specification

• • TLC: Thin Layer Chromatography

• • UV: Ultra Violet

6.0   PROCEDURE – CONTRACT LABORATORY AGREEMENT AND TESTING:

• • Procedure for approving the contract laboratory :

• • Head QC or designee shall audit the contract laboratory as per the “Contract Laboratory Audit Check List” Annexure -3 (but not limited to) and as per GLP guideline.

• • The auditor shall check the availability of instruments, qualification documents, and compliance status of other critical instruments like Polarimeter, Refractive index, Melting Point, etc. as per Annexure -3.

• • After completion of the audit, the audit report shall be prepared and submitted to the Quality Assurance with the comments.

• • Head QA shall review the audit report, containing observation/ deficiencies found during the audit and shall send the same to the contract testing laboratory within 15 days of audit, asking for compliance within one month of the audit report receipt.

                 Note: Any deviation from such a timeline shall be explained and justified.

• • Head QA shall ensure compliance of the audit query and shall approve the contract laboratory for the testing after confirmation of satisfactory compliance.

• • The quality agreement shall be signed only after confirmation of satisfactory compliance.

• • Audit of the contract laboratories shall be performed once in a two year or the frequency can be changed considering the no. of samples analyzed in contract laboratory or as and when required.

• • Every year contract testing laboratory shall provide the compliance of GMP.

• • The contract testing laboratory shall immediately inform in any noncompliance that occurs in the audit.

• • During re-qualification (re-audit) of the contract testing laboratory, in view of critical/ major/ minor observations found, the sample sending shall be stopped unless all critical/ major observations are complied by the contract testing laboratory.

• • Procedure for sending of samples to contract laboratory:

• • Sample for analysis shall be sent to the contract laboratory in case the analytical facility required is not available or the instrument which is required for particular testing is under maintenance or under any unavoidable circumstances etc.

• • Method transfer shall be performed to contract testing laboratory, in case of non-compendia method or in-house method is used for analysis.

• • The analyst shall prepare the “out lab test request slip” (Annexure-1) take the approval of the head QC or designee and shall send the test request slip along with the sample to the contract testing laboratory.

• • The analyst shall prepare the “Out lab test request” in duplicate and take the approval of the QC head or designee.

• • One copy of the “Outside lab test request slip” shall be sent to the out lab and the other shall be retained and kept as a record.

• • For the out lab test request slip, the “Slip No.” shall be assigned as follows:

• • • i.e. ABQC/OL//YYYY/XXX

                Where, ABQC stand for _<Company Short Name>, Quality control.

                 OL stands for out lab.

                 YYYY stands for the year (i.e. 2020)

                 XXX stands for serial no. (as 001)

Therefore, the first out lab test request “Slip No” for the year 2020 shall be as ABQC/OL/2020/001

• • The analyst shall make relevant entries in the “Out Lab testing register” (Annexure-2).  

• • The analyst shall pack the required quantity of sample in a suitable pack (As per material/product requirement) with proper labeling and identification and send along with the “Out lab test request slip” to the contract laboratory.

• • Some of the materials/products may require specific storage conditions and extra care while handling (e.g. liquid samples, light-sensitive, heat-sensitive, etc.).

• • Therefore a list of products/materials that are sent to out lab for testing shall be maintained along with their storage conditions etc. as pre Annexure-7 and shall be updated as and when required.

• • The sample shall be packed accordingly and sent to out lab for analysis.

• • The analyst shall provide the ATP and specification to the contract testing laboratory along with the sample.

• • ATP and specification shall be sent only once (In case of the same version) or as an when required.

• • The analyst shall ensure that analysis is performed as per the current version of ATP and specification.

• • ATP and specification shall be kept confidential and the contract testing laboratory shall return the superseding document on request to the company as a part of to retrieval of the circulated reference copies.

• • On request of contract testing laboratory for working standard, reference standard, impurity standard, reagent, chemical, column, etc. the required item shall be provided and shall keep record of the same.

• • After analysis contract laboratory shall send the analytical test report (COA) along with required raw data (like chromatogram, UV spectrum, histogram. etc.).

• • The COA shall contain as

• • • Name of product/material,

• • • Batch No/A.R. No.

• • • Sample analysis request No,

• • • Mfg. date,

• • • Expiry date,

• • • Specification no,

• • • Statement of compliance or non-compliance,

• • • Date and signature of designated qualified professional of contract testing laboratory.

• • The analyst shall make an entry in the “Contract testing laboratory register” for the “Received by/ Date” and make remarks in the “Remark” column if any.

• • The analyst/section head or designee shall review the COA and put the “Reviewed by” stamp with initials/date.

• • In case of any discrepancy, QC Head or designee shall coordinate with the contract testing laboratory to resolve the discrepancy.

• • COA can be acceptable through Email, fax, or scan for batch release purposes.

• • Hard copy/ approved electronic copy of COA and analytical data shall be reviewed on receipt.

• • The results sent by the contract testing laboratory shall be considered only when received through an authorized person.

• • Therefore the contract laboratory shall provide an approved list of their authorized personnel to company QA/QC along with their job description from whom the analytical results can be accepted.

• • The analyst shall enter the result and reference No. of COA in the analytical report.

Related: Analytical Data and Report Review Checklist

• • The COA and all raw data received from the contract testing laboratory shall be attached to the respective analytical reports for further review.

• • Handling of OOS results generated at contract laboratory:

• • During the contract laboratory audit, the auditor shall evaluate the OOS analysis SOP of the contract testing laboratory.

• • OOS analysis SOP of the contract laboratory shall be inline with the latest regulatory requirements and guidelines.

• • In case failure results observed at the contract laboratory then the contract testing laboratory shall immediately inform to sample provider.

• • The company shall ensure that investigation of failure shall be carried out at the contract laboratory in line with contract requirements.

• • The company shall provide support (column, reagent, working/ reference standard/ impurities, etc.) to the contract testing laboratory as and when required.

• • Based on the findings of the contract testing laboratory, Company shall decide the next step including re-testing or re-sampling or manufacturing investigation.

• • Based on the contract testing laboratory, plant investigation, and findings, QA Head or designee shall further decide the release status of the product/ material.

7.0   ANNEXURE – CONTRACT LABORATORY TESTING:

Annexure-1: Format for Out Lab Test Request Slip

Slip No:                                                                                                                             Date: Name of material/ Product Stage Raw material / In-process / Finished product / Stability samples /Microbiology samples/ Packing materials/ Water samples Additional information : Storage Condition Name of Manufacturer Name of Supplier B. No. A.R. No. Sample Qty. Mfg. Date: Batch Size Exp. Date: Test Required Test Reference/ Specification No. Name of Contract Laboratory Attachment (if any) Remarks (If any)       Sent by / Date:                                                                      Authorized by / Date:

Annexure-2: Format for Out Lab testing register

Slip No.	Date	Product/ Material	B. No. / A.R.No.	Test	Name of Contract laboratory	Received by/Date	Remarks

Annexure-3: Format for Contract Laboratory Audit Check List

Sr.No.	Check Point	Observations
1	Is the laboratory approved by Food and drug Administration (FDA)	Yes                         No
1.1	a) Last audit date	_ _ _ _ _ _ _ _ _ _ _
	b) Availability of compliance certificate	Yes                         No
2	Does the laboratory have the section for ?,	Yes                         No
	a) Chemical Analysis?	Yes                         No
	b) Microbiological Analysis?	Yes                         No
	c) Animal house facility?	Yes                         No
	d) Chromatography like HPLC, GC & IC..etc.	Yes                         No
	d) Any others ?	Yes                         No
3	Is the laboratory facility adequate for analysis ?	Yes                         No
4	Total number of employee in the laboratory.	_ _ _ _
5	Is the analyst academic qualification check ? If yes, Minimum Qualification:                               _	Yes                         No
6	Is job base qualification done ? If yes, check at least two analyst qualification record. Name of analyst-1 : Name of analyst-2 :	Yes                         No
7	Are the analysts experienced ? What is the ratio of experience Vs training ?	Yes                         No
8	Are there a training programme for analysis personnel ?	Yes                         No
9	Is their a list of persons who are authorized to provide the analytical result to the contract giver?	Yes                         No
	In their Job description available?	Yes                         No
10	Does the laboratory use chemicals/ reagents as per ATP report?	Yes                         No

 

Sr.No.	Check Point	Observations
11	Does the laboratory has adequate facility for the storage of Chemicals and solvents ?	Yes	No
12	Does the laboratory has adequate glassware cleaning procedure ?	Yes	No
13	Does the glassware washing procedure involve final rinsing of glassware with purified/ distilled water? Is it followed?	Yes	No
14	Is the glassware washing procedure validated ?	Yes	No
15	Does the laboratory use Class-A glassware for quantitative analysis ?	Yes	No
16	Does the laboratory use authentic procedures for reagent preparation, volumetric solution preparation and standardization ?	Yes	No
17	Does the laboratory use approved calibration programme/ plan ?	Yes	No
18	Are the laboratory instruments qualified as per USP classification system ?	Yes	No
19	Is there any preventive maintenance programme for instruments ?	Yes	No
20	Are the balances calibrated for operating & working range ?.	Yes	No
21	Does the laboratory use distilled water /purified water/ for the analysis purpose?	Yes	No
22	Is there a comprehensive procedure for storage and management of reference/ working standards?	Yes	No
	a) Is it adequate ?	Yes	No
	b) Is it followed ?	Yes	No
	c) Check any two WS/Reference standard/ impurity storage & reconsilation record.?	Yes	No

23	Is the quality of water used for analysis checked ? If yes.	Yes	No
	a) How frequent	_ _ _ _ __ _ _ _ _ _
	b) For which parameter	_ _ _ _ _  _ _ _ _ _ _
24	Does the laboratory uses Primary standard /Secondary standard/ Pharmacopoeial standard for the analysis of sample wherever required.	Yes	No
25	Does the laboratory use written procedure for the analysis of sample ?	Yes	No
26	Does the laboratory have adequate procedure for the receipt, registration, storage, analysis of samples and record, review, approval and report the analysis data and results ?	Yes	No
27	Does the laboratory have adequate system for the raw data handling ?	Yes	No
28	Does the laboratory have SOP for the OOS result investigation ?.	Yes	No
	a) Is in accordance with the plant SOP ?.	Yes	No
29	Does the laboratory have adequate facility for the document storage ?.	Yes	No
30	Does the laboratory have latest pharmacopeia available ?.	Yes	No
31	Does the microbiological section have basic facility like ?.	Yes	No
	a) Autoclave?	Yes	No
	b) Incubator?	Yes	No
	c) Laminar Air flow?	Yes	No
	d) Microscope?	Yes	No
	e) Colony Counter?	Yes	No
	f) Availability of microbial culture media ?	Yes	No
	g) Master culture ?	Yes	No
	h) Dry heat sterilizer ?	Yes	No

 

Sr.No.	Check Point	Observations
32	Does the microbiology section sufficiently equipped for the BET/LAL testing ?	Yes	No
	a) LAL testing tubes ?	Yes	No
	b) Lysate ?	Yes	No
	c) Control standard Endotoxins ?	Yes	No
	d) Incubator for LAL test ?	Yes	No
	e) LAL reagent water ?	Yes	No
33	Does the microbiology section have sufficient facility for performing ?	Yes	No
	a) Sterility testing ?	Yes	No
	b) Microbial Limit test & Bio assay.	Yes	No
34	Is the animal house sufficiently facilitated for Pyrogen test?	Yes	No
35	Is the animal house sufficiently facilitated for Toxicity test?	Yes	No
36	Does the laboratory issues adequate certificate of analysis ?	Yes	No
37	Is there any raw data retention policy ?	Yes	No
38	Is there any policy of data backup ?	Yes	No
39	Is there any group policy applied for analysis on instruments.	Yes	No
40	Is the instruments used for analysis, in compliance of 21 CFR ?	Yes	No
41	Is there an electronic audit trail generated ?	Yes	No
42	Does electronic audit trail review by reviewer ?	Yes	No

 

Sr.No.	Check Point	Observations
43	Is the general pharamacopoeial method used for testing validated ?	Yes                         No
44	Is method verification performed for compendia method ?	Yes                         No
45	Is method validation/ transfer required ?	Yes                         No
46	Is the laboratory having system for SOPs and documentation control?	Yes                         No
47	Is the laboratory having procedure for Hygiene and Safety ?	Yes                         No
48	Is the laboratory having procedure of disposal ?	Yes                         No
49	Is the laboratory having Quality Manual ?	Yes                         No
50	Is contract testing laboratory used NIST traceable standard for calibration and standardization ?	Yes                         No
51	Is all calculation done by validated software ?	Yes                         No
52	Is there any procedure on how long to records ?	Yes                         No
53	Is there any procedure for self inspection or audit.	Yes                         No
54	Are self inspection or audit observation documented?	Yes                         No
55	Is our own analysis raw data checked during re-audit ?. If yes, Product Name : Batch No/A.R.No. :	Yes                         No
56	Is any OOS/ deviation happened at contract testing laboratory from previous audit & reviewed ?. If yes, Product Name : OOS /Deviation No. :	Yes                         No
57	Is SOP of out of calibration (OOC) available. If yes, please note one instrument name and test of OOC. Instrument Name : OOC No/ Test:	Yes                         No

Remarks:____________________________________________________

Date of Audit
Audittee	Name	Designation	Signature
Audited By

Opinion: Based on the survey of the laboratory———————-, it is recommended that, the laboratory qualifies/does not qualify for analysis of the sample.

Annexure-4: Format for Agreement for Contract Analysis

Contract giver  :	Contract acceptor :
<Company Name>	<Contract Laboratory Name>
<Company Address>	< Contract Laboratory Address>
Tel. No.: ………………………	Mobile No. +91………………………
Fax No.: ………………….	Extn. : …….
Email:………………………………………	Email: …………………………………

• Scope:

• • This contract is applicable for the samples send by ………………… to  (referred to as  “…….. ” hereafter in the contract) for the testing.

• Sampling:

• • The ………… shall collect the sample as per ……… SOP for relevant material and send the part of sample required for carrying out particular analysis to ….. with proper labeling & complete information of sample (e.g Product name, Batch No./A.R. No., Date of manufacturing, Expiry date and Manufacturer’s name, etc.)

• Document: 

• • The ………… must ensure that every sample accompanies all necessary documents e.g. sample analysis request, Instructions (if any)——— may return the received samples if required documents not accompanying with samples.

• • The …………. shall ensure that the required & relevant information like Product/Material Specification, Analytical testing procedure relevant to the sample is either available or shall be made available to the contract acceptor at the time of analysis and need to confirm as suitable for the use in the context of the contract laboratory.

• • Pharmacopoeial references for the analysis shall be mentioned in case if pharmacopoeial limits & methods of analysis to be followed.

• • The …………… Shall ensure that the current version of documents is provided to the contract laboratory…………….. shall return the superseding document on request from………….. in the process to retire the circulated reference copies.

• • ……… will submit the results in the form of a certificate of analysis or compliance slip and raw data (if applicable) with their references no. for traceability of analytical raw data.

• Responsibilities:

  • For …… (Contract testing laboratory)  shall be responsible for:

• • Providing adequate facilities and qualified staff with relevant experience to carry out necessary analysis/ testing as per current GMP/GLP practices.

• • Carrying out the analysis as per specification and ATP provided by …………… No change in the specification or ATP shall be done by………

• • ………. shall inform ……………. for any deviation / Out of specification (OOS) results within 24 hours of OOS results generation……………………. shall proceed further investigation as per the intimation received from …………………

• • Investigate the Out of specification (OOS) results as per respective SOP and share the finding along with data to ……………. for further action.

• • Submit the results, in form of a report duly signed by an authorized person. The report shall bear a reference no. by which analytical raw data can be traced at ……….

• • Do not send the sample to the same or other testing laboratories for analysis purpose.

• • ……….. shall inform ……………….. in case of any non-compliance of regulatory

• • For ……………………(Company) shall be responsible for :

• • Evaluation for the impact of any deviation / OOS result informed by, and intimate to………….. for further course of action.

• • ………………. shall have the final authority of accepting or rejecting the product/material based on the results given by ………….

• • ………………. shall provide the reference/ working standard/ impurity standard, any specific reagents……etc on request of…………, in case of reference/ working standard/ impurity standard, any specific reagents, etc. are not available with ………….,

• Confidentiality:

• • ………. shall maintain the documents and information submitted by ………….. as confidential and shall not pass to any third party/ unauthorized agency/ company.

• Audit:

• • The periodic audit shall be carried out by a representative from ………….. once in two years or as and when required and audit report shall be provided to……………………………………………………. for further action and compliance.

• Annexure-6:         – List of materials for out -lab testing …………… – List of tests to be performed at ……….

(Note: The revision of the Annexure-6 will be independent of the contract, which will not require the contract to be revised & re-signed.)

• Agreement valid up to: DD/MM/YY to    DD/MM/YY

• Agreement: 

  • We confirm that all the information contained in this document will be confidential and we are in agreement with the terms and conditions described in the above contract and shall abide by those.

• • If any amendment is necessary for the future it may be done by mutual consent.

For …………………………….	For ……………………………………….
Address : Name : Designation : Sign/Date:	Address : Name : Designation : Sign/Date:

Annexure-5: Format for Contract Laboratory Audit Form

Name of the laboratory: ………………………………

Address: ………………………………………………………………

Tel No……………………..

Email:………………………………..

Primary contact: For Sophisticated Instrumental Testing of Raw Material, Finished Products, Stability samples, Water samples, Microbiology samples, and Packing materials.

Telephone/Fax/E-mail : +91-…………………………..

Audited for: For Sophisticated Instrumental Testing based sample of Raw Material, Finished Products, Stability samples, Water samples, Microbiology samples, and Packing materials.

Reason for audit: As per regulatory requirement

Date of audit                 :

Auditor(s)                       : Name,  Designation:

Site representative          : Name, Designation

Annexure-6: Format for List of materials for out lab testing

Sr. No.	Name of Material	Name of Test	Reason for sending

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