SOP For Good Laboratory Practices

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SOP For Good Laboratory Practices

1.0. OBJECTIVE
1.1 To lay down a procedure for Good Laboratory Practices in Quality Control Laboratory.

2.0. SCOPE
2.1 This procedure is applicable Good Laboratory Practices in Quality Control Laboratory

3.0. RESPONSIBILITY
3.1 QC Officer or QC Executive

4.0. ACCOUNTABILITY

4.1 QC Manager

5.0. DEFINITION:
Good Laboratory Practices or GLP is a set of standards proposed to guarantee the quality and

integrity of non-clinical laboratory studies that are expected to support research or marketing permits for products

6.0 PROCEDURE:
6.1 .1 Use the current specifications, STP, SOP and protocols.
6.1.2 Record the raw data online in the issued check list.
6.1.3 Check the instrument calibration validity before start of analysis.
6.1.4 Data shall be written and verify according to I.P./B.P./U.S.P/I.H.S.
6.1.5 Attached the Print outs with raw data of analysis with weight slips, chromatographs etc.
6.1.6 If report is Out of specification, out of calibration, incidents deviations or any abbrevent result, report
to QC Head.
6.1.7 For analysis, use clean and dry glassware.
6.1.8 The glasswares used for analysis should be marked with minimum details as batch number for
identification and detectability with analyst sign.

6.1.9 Dry or clean the burette and pipette with a tissue paper before dispensing the withdrawn liquid.
6.1.10 After analysis, remaining sample should be discard.
6.1.11 Work in fuming hood if sample is odor or fume releasing.
6.1.12 Use purified water or WFI for testing, as per specification.
6.1.13 Handle hazardous materials as per the material safety data sheet (MSDS).
6.1.14 Record instrument log books with sign and date.
6.1.15 Correction of writing mistakes shall be done by single line cut with signature and date, same shall be
justified with proper short remark.
6.1.16 During laboratory operations, use Personnel Protective Equipment’s (PPE’s).
6.1.17 Spillage of solution on the work bench should be avoided or if any spillage occurs, informed to
Section Incharge.
6.1.18 Funnel should be used to transfer the titrant to a burette.
6.1.19 Glasswares should be scratches and stains free.
6.1.20 Do not leave any glassware unattended if heating is carried out.
6.1.21 Do not add water in glassware containing concentrated acid as may explode. Always take some
water in the glassware and then add concentrated acid slowly with cooling.
6.1.22 Check all the instruments should be under calibration.
6.1.23 Do not use Scrap paper, sticky notes, tissues or other unofficial sheets for writing the
observations.

6.1.24 Do not practice blowing of pipettes by mouth.
6.1.25 Use of eraser or white ink should be inhibited.
6.1.26 Don’t mix up glassware at one place.
6.1.27 Usage of damaged syringes and syringe having scratches and stains should be inhibited.

6.2 Weighing practice:
6.2.1 Ensure that balance is calibrated before starting the weighing activity.
6.2.2 The balance and the surrounding area should be clean.
6.2.3 Ensure to weigh quantity as mentioned in respective procedure and take print out.
6.2.4 Ensure the label affixed on product or material bag to be weighed and marking on

glassware before initiation of weighing.
6.2.5 Liquid spillage inside the balance must be strictly avoided as it can cause serious

damage to the balance and they may be difficult to remove.

6.2.6 Do not return any excess material to the original container. Excess material must be disposed off in the waste bin.
6.2.7 All standard weights and sample weights (or volumes if the standard or sample is liquid) should be recorded
and the printouts of weights should be attached with raw data of analysis.
6.2.8 The impurities and reference standards are available in less quantity, the weighing of impurities and
reference standard can be reduced provided that, final concentration of solution should be prepare as per
STP.
6.2.9 Maintain sample and standard solutions under protective conditions, if indicated in analytical test procedures,
such as light sensitive.
6.2.10 Before handling the instrument, ensure that it should be clean.

6.3 Handling of Volumetric Flask

6.3.1 The volumetric flask should be leveled up to the mark and calibrated.
6.3.2 The lower and upper meniscus should be appropriately considered for different types of solvents. For solvents
like Methanol, Acetonitrile, Tetrahydrofuran, Purified water, the lower meniscus should be considered. For
colored solutions, the upper meniscus should be considered.
6.3.3 Whenever any part quantity of solvent is poured into the volumetric flask and shaken, then the volume should
be made after some time till the solvent contracts to its original volume.
6.3.4 The volumetric flask should be stoppered using properly fitting stopper.
6.3.5 Do not use volumetric flasks having scratches or marking is not clearly visible or if the

capacity of volumetric flask printing is not visible.

6.4 Handling of Burette
6.4.1 Suitable burette should be used in different titrations considering the burette reading.

For a burette reading ranging about 10 to 20 ml, a burette with 25 ml capacity should be used.

Similarly for a burette reading ranging about 1.0 to 9.0 ml, a burette with 10 ml capacity should be used.

6.4.2 The burette should be rinsed with purified water 1-2 times and then with the volumetric

solution titrant. In case of non aqueous, burette does not rinsed with purified water,

it should only be rinsed 1-2 times with the volumetric solution titrant.
6.4.3 The lower or upper meniscus should be properly considered for different types of solutions.

For transparent volumetric solutions, the lower meniscus should be considered. For colored

volumetric solutions, the upper meniscus should be considered.
6.4.4 Do not use burettes having scratches or any kind of stains or the marking is not clearly visible or solution is
leaking from the tip.

6.5 Handling of Volumetric Pipette
6.5.1 The volumetric pipette contains the delivered volume as the specific volume of the capacity.

When 1.0 ml volumetric pipette is used, and afterward the volume which it delivers out from

the pipette is actually equivalent to 1.0 ml. The amount of solution remaining in the pipette

should not be forced to remove from the pipette.
6.5.2 The volumetric pipette should be leveled up to the mark and should be calibrated.
6.5.3 The lower or upper meniscus should be properly considered for different types of solutions.

For transparent solutions, the lower meniscus should be considered. For colored solutions,

the upper meniscus should be considered.
6.5.4 During transfer of volume, the pipette should be held at a degree of about 30° touching

the tip of the pipette to the inner wall of the volumetric glassware.
6.5.5 Do not use volumetric pipette having scratches or any kind of stains or the marking is not

clearly visible or the tip is broken.
6.5.6 Volumetric pipettes are used for the transfer of Standard and sample solution and dilution, for

the analysis of Limit test, for the Volumetric solution preparation.

6.5 Handling of Measuring Cylinder
6.5.1 Suitable measuring cylinder should be used in different tests considering the volume. For volume

ranging from 10 to 20 ml, a cylinder with 10 ml or 25 ml capacity should be used as appropriate.
6.5.2 The lower or upper meniscus should be properly considered for different types of solutions. For

transparent solutions, the lower meniscus should be considered. For colored solutions, the upper

meniscus should be considered.
6.5.3 Do not use cylinder having scratches or if the marking is not clearly visible.

6.6 Handling of instruments
6.6.1 Instruments should be calibrated before use.
6.6.2 Instruments should be identified with sequential identification number.
6.6.3 Instruments should be calibrated and maintained as per the respective calibration procedure

and schedule and the calibration status of the instrument should be displayed on the instrument.
6.6.4 Calibration and preventive maintenance of laboratory instruments should be performed as per the pre-defined schedule.

6.7 Work allocation and Good Documentation Practices
6.7.1 Executive or officer should allot the work as per priority of the material or first come

first analysis basis.
6.7.2 After completion of analysis, the analyst shall update the status of analysis in respective

material inward register and log book.
6.7.3 Executive or officer should review the analytical documents, chromatograms;

weight slips etc and should generate COA.
6.7.4 The analytical raw data should include the sample details, the references of standard

observations for the particular test, printouts of the chromatograms.
6.7.5 All the data should be recorded in the respective logbook and raw data sheet.
6.7.6 All raw data should be identified by the product or material name and the batch

number or analytical report number.
6.7.7 All recorded data should be signed with date by the analyst and should be checked by the executive.
6.7.8 All numerical data should be clearly labeled with headers identifying the data and

must have the unit of measure specified.
6.7.9 All data should be online recorded accurately. The calculations can be done after

completion of the analysis.
6.7.10 Analyst should enter the result in the validated software after completion of the analysis.
6.7.11 In case, the respective person is on leave, pending results entries can be assigned to

the other analyst and the results can be entered in software.
6.7.12 Raw data should have cross reference of batch number and valid up to of the working standard used,
batch number of the volumetric solution used and column number used during analysis.
6.7.13 In case of sequential analysis, the data should be kept along with one analytical reports and

cross reference should be given in other reports for traceability.
6.7.14 All original generated data including printouts, and other original documentation must

be retained, even if the data is not utilized.
6.7.15 Overwriting should be avoided. Any cancellation should be done by strike out by single

line, put signature and date, write the correct value or letter beside the wrong value or letter.

The corrected figure or letter should be readable.
6.7.16 Blank spaces during the raw data recording shall be crossed out and labeled as Not Applicable (NA).

6.8 Handling of standard and sample preparations
6.8.1 Sample solutions and all related glassware should be retained until completion

of review of the results.
6.8.2 Remove all used glassware from workbenches and send for washing after the review of

the results and after any investigation.
6.8.3 Handle one product at a time. Work area should be clean and tidy to avoid cross contamination.
6.8.4 In case of spillage of solution, breakage of glass apparatus which hold the solution during

the analysis or due to any assignable cause which analyst came to know while preparation

of solution and the same should be recorded into raw data, should be immediately informed

to QC manager. After proper investigation, executive should issue the additional continuation

sheet for that particular test.

6.9 Handling of Reference standard and Working Standard
6.9.1 Use only current lot of reference standard or working standard.
6.9.2 While using the reference standard or working standard, carefully transfer the

quantity required for the analysis without altering the potency of the reference standard.
6.9.3 If moisture content or loss on drying to be performed on the standard, perform on the

day of use before evaluating the potency.

6.10 Good Chromatographic practices
6.10.1 HPLC analysis vials should be label using a legible marker pen in an identifiable manner.
6.10.2 Use fresh vials for HPLC analysis.
6.10.3 HPLC vials should not be overfilled. HPLC vials should be filled up to 80% of the capacity of the vial.

Overfilled vials may affect injection accuracy and precision.
6.10.4 Rinse vials with a little volume of the solution that is being filled into the vial before to final filling.
6.10.5 If Similarity factor between two standards is not achieved, then do not continue the analysis.
6.10.6 If peak splits or the improper peak is observed or the leakage from column is observed, then

uncontinue the analysis.
6.10.7 Do not shutdown HPLC directly when it is connected through software.

6.11 HPLC Column Washing
6.11.1 During analysis, analyst should log in into HPLC system using his or her individual login name and password
6.11.2 After completion of sequence injection , HPLC column washing should be done.
6.11.3 The column washing programme should be included in each injection sequence and the injection

sequence should be verified by the reviewer, after verification the analysis should be started and

the printout should be attached with raw data of analysis.
6.11.4 Always keep the chemicals in closed condition during sample preparation.

6.12 Deviations and Investigations
6.12.1 If any incidence to methods, dilutions, solution preparations are made, the details

should be entered to the record.
6.12.2 All aberrant results, OOS investigations must be performed and documented according to SOP.
6.12.3 All aberrant results, OOS and any discrepancy observed in the analytical data or records

should be brought to the immediate attention of the QC Manager.

6.13 Stability study
6.13.1 Stability of a Pharma product means how long it can maintain its original form without any

visible changes under the influence of various environmental factors like temperature, humidity, light
6.13.2 Determine the time during which a product meets registered standards when stored

under conditions ( called as accelerated study). To show that the product remain within its expiry

specification throughout its proposed shelf life (called as real time study).
6.13.3 Stability study is to be followed as per SOP for Stability Studies of finished products.
6.13.4 A description of the storage conditions for all stability samples, includes temperature,

relative humidity and sample storage condition.
6.13.5 A requirement that the drug product is stored in the same container closure system in

which it is marketed (accelerated or real time )
6.13.6 An adequate number of batches of each drug product should be tested to determine an

appropriate expiry date and a record of such data should be maintained.
6.13.7 Any stability testing failure requires to be properly investigated through OOS or incident

document. It will include a root cause analysis investigation, corrective and preventive actions.
6.13.8 The conclusions of the investigation should be approved by the quality control department,

with final approval by the Quality assurance department.

6.14 Generation of Password and Password policy
6.14.1 Passwords are an important aspect of security for computer, instrument, equipment. They are

the protection for User and system accounts. Administrator privileges, login and password for all

instrument or equipments, are assigned to IT Head.
6.14.2 Date and time should be locked in all critical instruments which include, but not limited

to HPLC, FTIR, UV, analytical balance. Privilege to change date and time in instruments or equipments lies

with administrator, who is an IT Head.
6.14.3 Every user should have separate ID and password for an account.
6.14.4 Password should be re-defined as, User password is disclosed by anyone, forgot

the password, locked passwords after invalid attempts, if software is re installed, users

will change their password whose password is due, if the users forgot to change the password

after expiry he will change the password in consultation with administration.
6.14.5 Do not share the password to anyone.

6.15 Data integrity requirements
6.15.1 Qualification, Validation and Verification of instrument, equipments and software

should be fit for the intended purpose.
6.15.2 All the used documents and methods should be approved.

7.0 ABBREVIATIONS

Sr. No.	Abbreviation used	Extended Form
1.0	OOS	Out Of Specification
2.0	QC	Quality Control
3.0	QA	Quality Assurance
4.0	SOP	Standard Operating Procedure
5.0	STP	Standard Testing procedure
6.0	HPLC	High Performance Liquid Chromatography
7.0	FTIR	Fourier Transform Infrared Spectroscopy
8.0	UV	Ultraviolet-Visible Spectrophotometer