Bio Analytical Sop

STANDARD OPERATING PROCEDURE

TITLE: Recording of Raw Data in Bioanalytical Laboratory

SOP NUMBER: SOP-BAL-004-00

VERSION: 00

SUPERSEDES: N/A

ISSUE DATE:

EFFECTIVE DATE:

REVIEW PERIOD: 2 years

DISTRIBUTION AREAS:

PREPARED BY REVIEWED BY APPROVED BY AUTHORISED BY

NAME

DESIGNATION

SIGN & DATE

Distribution Details:

Copy No.: Location:

Amendment Details:

Amendment Effective Date1 2 3

VERSION NO.

EFFECTIVE DATE

REASON FOR REVISION

1.0 OBJECTIVE

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To describe a procedure for recording of raw data using various forms during the conduct of a project in bioanalytical department.

2.0 SCOPE

Applicable to all projects performed in bioanalytical department to ensure GLP compliance and traceability.

3.0 RESPONSIBILITY

All the analysts along with group leader involved in the project are responsible for the compliance and implementation of this SOP.

4.0 DEFINITIONS AND ABBREVIATIONS

SOP : Standard Operating Procedure

QA : Quality Assurance

OECD : Organization for Economic Co-operation and Development

CC : Calibration Curve Standards

QC : Quality Control samples

DF : Deep Freezer

FRZ : Freezer

GLP : Good Laboratory Practices

Raw Data : Raw data means all original test facility records and documentation, or verified copies thereof, which are the result of the original observations and activities in a study. Raw data also may include, for example, photographs, microfilm or microfiche copies, computer readable media, dictated observations, recorded data from automated instruments, or any other data storage medium that has been recognized as capable of providing secure storage of information for a time period as stated in respective study plan or protocol or in-house SOP.

5.0 PROCEDURE

5.1 Get all the enclosed serial numbered raw data forms issued from QA.

5.2 All the raw data forms required for each study must be requested as soon as the protocol / SOP is approved for that project and the raw data forms required for activity such as qualification / calibration must be requested well in advance before the due date. Additional forms can be obtained during the project / activity, as and when required.

5.3 Fill all the raw data forms in black ink.

5.4 The individual should record all the data generated during the conduct of the project / activity directly, promptly, accurately, and legibly.

5.5 Strike off any wrong entry with a single line across the entry, incorporate the correct entry followed by initials and date. If there is insufficient space near the ‘raw data change’ indicative symbols such as asterisk with a footnote may be used.

5.6 Cancel any blank space of a page with a single stroke diagonally. Write NA for not applicable.

5.7 All the analysts involved in a particular project and concerned to the particular activity must fill up the necessary raw data forms, sign and date them as soon as the activity is over.

5.8 When the raw data is in the form of a print out (e.g. weighing slip), paste the weighing slip on raw data forms and sign the print out preferably in such a way that the signature and date spreads from the weighing slip on to the raw data form.

5.9 Preferably record all the dated with format DD/MM/YYYY.

5.10 The group leader, involved in a particular project, is responsible for verification of all the information in each documented raw data forms of corresponding project. The group leader is responsible for verifying the activity preferably within 3 days after the completion of the activity by signing at the space provided (Reviewed by) while checking the following:

- Accuracy, completeness, consistency and traceability.

- Non-computerized calculations.

- Compliance to relevant SOP’s

5.11 Attached (Form Number 1-11) are formats of raw data forms. Any modifications of these forms are strictly prohibited. Cancel all blank / unused forms and file them in their specific project files.

5.12 Do not use whitener, blades and tapes to correct the data

6.0 DESCRIPTION OF RAW DATA FORMS

6.1 Study Personnel (Form Number 1)

6.1.1 Complete this form at the initiation of every project. Record signature and initials of all the analysts along with group leader involve in a project stating their functions. Incorporate the details in this form as and when a new personnel gets involved in a project.

6.2 Instrument Identification and Chromatographic Conditions (Form Number 2)

6.2.1 Record the Instruments identity and conditions to be employed during the course of the project. Complete this form in accordance with the conditions mentioned in the protocol / method SOP.

6.3 Stock Weighing and Stock Preparation (Form Number 3)

6.3.1 Complete this form after preparing stock solution of the analyte(s) and / or internal standard.

6.3.2 Provide chemical properties, batch number, manufacturing details along with the date of preparation and date of expiry of the stock solution, storage condition and identification of the storage area. In case of method validation, also provide the identification of stock solution kept for stock solution stability exercise, its storage condition and the identification of the storage area. Assign a unique ID no. to each stock solution.

6.3.3 Attach the printout of weight measurement to the form with signature and date.

6.4 Sample Processing Sheet (Form Number 4)

6.4.1 Complete this form to document the extraction of analyte(s) from each biological matrix for each validation / analytical batch.

6.4.2 Document the extraction technique adopted during the sample preparation for chromatographic analysis.

6.4.3 Record the details of kits (solid phase extraction, ultra filtration etc.), reagents and solvents used for sample processing.

6.4.4 Document SOP No. / Validation protocol No. in the reference.

6.4.5 Document the identification of subject sample, calibration curve standards and quality control samples that are to be processed.

6.4.6 Record the time of retrieval of the samples from deep freezer and processing starts time etc.

6.4.7 All the analysts involved in the processing should sign the form. Each activity during the extraction procedure should be self verified by the respective analyst performing the activity and in addition the form documentation should be verified by group leader. An example of the sample processing log has been provided, however the sample processing log will differ from project to project and the format of the extraction procedure will be given in the respective protocol / SOP. The format given in protocol / SOP will be issued by the QA.

6.4.8 Document the IDs of missing samples, if any, lost during processing or have insufficient sample volume to enable processing. Document the dilution factor used in this form, in case, samples are diluted for processing.

6.4.9 Record the processing start time, end time and time of transfer of samples to the auto injector. Document the instrument in which samples are being loaded, along with the ID of the mobile phase being used for that analysis. In case, the processed samples are stored prior to their transfer to auto injector, then record the identification of the interim storage area and storage conditions. Use one form to record the processing of one analytical batch.

6.5 Solution Preparation (Form Number 5)

6.5.1 Complete this form to record the details of the preparation of each solution or reagent, (e.g., mobile phase, buffers, acid solutions and rinsing solution etc.).

6.5.2 Assign a unique ID number to each solution.

6.5.3 Attach the print out of weighing, wherever applicable.

6.6 Stock dilution (Form Number 6)

6.6.1 Complete this form while preparing dilutions from the standard stock solutions. Record the dilution procedure stepwise. Give a unique ID number to each dilution. .

6.7 Preparation of Spiked Calibration Curve Standards / Quality Control Samples (Form Number 7)

6.7.1 Complete this form to record the details of additions of diluted stock solutions to biological matrix (blood, serum, plasma or urine) for the preparation of spiked calibration curve standards or quality control samples or any other spiked samples. Maintain constant ratio of spiking solution to the biological matrix in all samples.

6.8 Sample dilution (Form Number 8)

6.8.1 Complete this form when a sample needs dilutions. Give information regarding matrix, volume of sample and the dilution factor.

6.9 Reintegration (Form Number 9)

6.9.1 Fill the reintegration form, when one or more of the chromatograms in a run are manually integrated or reintegrated using integration parameters that are different from the rest of the chromatograms within the same batch / run. Get approval from Head of the department / Group leader for reintegration.

6.10 Reinjection (Form Number 10)

6.10.1 Fill the reinjection form, when one or more of the samples were reinjected due to following discrepancies.

Batch stopped due to system error Vial skipped

6.11 Memo to file (Form Number 11)

6.11.1 Fill this form to record any additional information or unanticipated occurrence during a project.

7.0 REFERENCES

7.1 OECD Principles of Good Laboratory Practice (as revised in 1997). Series on Principles of Good Laboratory Practice and Compliance Monitoring, No. 1. OECD Environmental Health and Safety Publications. Environment Directorate, Organisation for Economic Co-operation and Development, Paris 1998. ENV/MC/CHEM (98)17.

8.0 ATTACHMENTS

8.1 Form Number 1: Study Personnel

8.2 Form Number 2: Instrument Identification and Chromatographic Conditions

8.3 Form Number 3: Stock Weighing and Stock Preparation

8.4 Form Number 4: Sample Processing Sheet

8.5 Form Number 5: Solution Preparation

8.6 Form Number 6: Stock Dilution

8.7 Form Number 7: Preparation of Spiked Calibration Curve Standards / Quality Control Samples

8.8 Form Number 8: Sample Dilution

8.9 Form Number 9: Reintegration

8.10 Form Number 10: Reinjection

8.11 Form Number 11: Memo to File

Form Number 1

Study Personnel

Project No.: Analyte Name (s):

SOP No. / Protocol No.:

S. No. Name Activity Signature Initials Date

Form Number 2

Instrument Identification and Chromatographic Conditions



Additional Instruments/Column used:

Chromatographic Conditions

Instrument ID: Column ID:

Detector:Software and Version:

Column specifications:

Mobile phase:

Injection Volume: Flow rate (ml/min):

Column Oven Temperature:Autosampler temperature:

Wavelength or Mass transaction for analyte(s):

Wavelength or Mass transaction for IS:

Completed by Date

Reviewed by Date

Other Instruments

Shaker ID: Centrifuge ID:

pH Meter ID: Evaporator ID:

Analytical Balance ID: Microbalance ID:

Refrigerators ID: Vortex Mixer ID:

DF / FRZ ID:Positive Pressure Unit ID:

Completed by Date

Reviewed by Date

Instrument/Column ID Date of first use Completed by Reviewed by

Form Number 3

Stock Weighing and Stock Preparation



Name of Reference Standard:

Source / Supplier: Lot No./ Batch No.:

Date of Manufacture / Effective Date:

Date of Expiry / Revalidation Date:

Molecular Weight of Compound:

Molecular Weight of Free Compound:

Amount Weighed: Volume made up:

Solvent used: Solvent Batch No:

Balance ID:Purity of Reference Standard:

Concentration of Stock:

Show Calculations

Light Sensitive (Y/N): Storage ID:

Stock solution ID:

Date Prepared: Expiry Date:

Stability exercise aliquots:

Stability stock ID: Storage ID:

Remarks:

Prepared By: Reviewed By:

Date: Date:

Form Number 4

Sample Processing Sheet



Internal Standard ID:

Mobile Phase ID: Instrument ID:

Parameter:

Extraction Method:

Kit / Cartridge: Batch No.:

Pipette(s)ID:

Subject ID: Period ID:

CC ID: QC ID:

Sample withdrawal time: DF / FRZ ID:

Processing Start Time: Processing End Time:

Time of Transfer to Auto injector:

Interim Storage, If any:

Storage ID: Storage Location:

Reagent/ Solvent/ Solution used Batch No. Expiry Date

ID(s) of Missing / Lost / Insufficient / Diluted samples:

Page 1 of 2

Form Number: 4 (Contd…..)

(The below mentioned format is just an example)

1. Thaw the samples to room temperature.

2. If any solid material is noticed in the plasma sample, centrifuge the same before aliquoting.

3. Take 100 µl of plasma sample into RIA vial.

4. Add 25 µl of IS working solution.

5. Add 10 µl of 10 % formic acid.

6. Vortex using a cyclo-mixer (about 5 seconds).

7. Add 2.5 ml of DEE:DCM.

8. Shake (vortex) the samples on a shaker at 2500 rpm for 5 minutes. Allow the layers to separate.

9. Transfer 2 ml of the organic layer into a separate glass test tube.

10. Evaporate to dryness by using an evaporator under nitrogen at about 40°C.

11. Reconstitute the sample residues in 1 ml of the ‘dilution solvent’.

12. Transfer the solutions into autosampler vials and place the vials in the auto sampler.

Remarks:

If more than 1 person is involved in the processing then that person should sign besides the respective box.

Processed By: Reviewed By:

Page 2 of 2

YES/NO

YES/NO

YES/NO

YES/NO

YES/NO

YES/NO

YES/NO

YES/NO

YES/NO

YES/NO

YES/NO

YES/NO

CONFIDENTIAL

Form Number 5

Solution Preparation



Storage ID: Shelf Life:

Name of Solution:

Date Solvent / Reagent

Batch No. Pipette(s) ID

Volume / Weight

Final Volume

(ml)

pH Solution ID Signature and DatePrepared

ByReviewed

By

Remarks:

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CONFIDENTIAL

Form Number 6

Stock Dilution


SOP No. / Protocol No.: Solvent used:

Purpose / activity:

Date Stock ID Stock Conc. Stock Volume

Diluted to /

Volume of solvent added

Pipette ID

Batch Number of the solvent

Final Con. Prepared dilution ID

Signature and DatePrepared

byReviewed

by

Remarks:

Author: _________________________ (Sign & Date) of 19

CONFIDENTIAL

Form Number 7

Preparation of Spiked Calibration Curve Standards / Quality Control Samples

Project No.: Analyte Name (s):SOP No. / Protocol No.:

Activity: Pipette ID(s): Volume of each aliquot:

ID of matrix lots: Individual Matrices Plasma Lots used for pooling: Pooled Matrix ID: Matrix: Serum/ Plasma/Blood/ Urine: Anticoagulant:

Stock ID Stock Conc. Stock Volume

Matrix Volume

Total Volume

Standard / QC Conc.

ID of Standard / QC No. of Aliquots

Storage ID: Storage Date & Time:

Prepared By: Reviewed By:

Remarks:

Form Number 8

Sample Dilution


CONFIDENTIAL



Date Sample ID Blank Matrix ID Sample Volume

Matrix Volume

Total Volume Dilution Factor

Signature and Date

Prepared By Reviewed by

Remarks:


Form Number 9

Reintegration



Instrument ID:

Date Sample ID Reason for ReintegrationSignature and Date

Requested by Approved by

Remarks:


Form Number 10

Re-injection



Instrument ID:

Date Sample IDFirst

injection date

Reinjection date

Reason for Reinjection

Sign and DateRequested

byApproved

by

Remarks:


Form Number 11

Memo to File



Performed by: ____________________ Date: __________________

Reviewed by: ____________________ Date: __________________


Bio Analytical Sop

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