Instruction for washing of HPLC columns

1.0     Purpose     :      To provide an instruction for washing of HPLC columns.

2.0     Objective   :      To provide a documented procedure for washing of HPLC columns.

3.0              Scope      :     This procedure is applicable for washing of HPLC columns in QC Department ---Pharmaceuticals Ltd, Ankleshwar.

4.0      Responsibility   :

·        Primary  :    QC Chemist / QC-Officer

·        Secondary  :  Overall QC – In charge

5.0       Procedure  :

·        After completion of analysis stop the pump, keep the reservoir in the distilled & filtered water.

·        Open the purging valve of the pump; purge the system for 3 to 5 minutes to remove air bubbles. Close the purging valve by decreasing the flow rate up to zero.

·        Wash the HPLC column initial with HPLC grade water for about 15-20 minutes.

·        Then wash the HPLC column with respective solvent mixtures (e.g. 50:50 Methanol: Water or Acetonitrile: Water) for minimum ½ hr to 1 hr.

·        Finally wash the HPLC column with respective solvent (Acetonitrile / Methanol) for about 15-30 minutes.

·        Keep flow rate 0.5 ml / min or 1.0 ml / min. increase flow rate gradually.

·        Check the pH of eluent on pH paper (it should be neutral) 

·        Store the HPLC column in solvent (acetonitrile or methanol).

·        Disconnect the HPLC column and keep it at respective column storage box.

·        Maintain the cleaning record in HPLC column logbook.

6.0      Reference Document  :

v      HPLC column use logbook.

Log Book For HPLC Column

Column ID.

:

Product

:

Date	Sample ID	Batch No.	Mobile Phase	No. of Inj.	Washing Time		Storage	Pressure	Analyst	Remarks
					From	To
Format:-F/QC/013

Re-Testing of Raw materials

1.0         Purpose   :     To provide an instruction for re-testing of raw materials and intermediates.

2.0         Objective   :   To provide a documented procedure for re-testing of raw materials and intermediates.

3.0             Scope       :   This procedure is applicable for re-testing of raw materials and intermediates in QC department of --------Pharmaceuticals Ltd,Ankleshwar.

4.0         Responsibility  :

·       Primary   : QC Chemist / QC Officer

·       Secondary : Overall: QC – Incharge

5.0       Procedure:

·        After the receipt of re-testing intimation note from store department, QC Chemist takes its entry in the respective Re-testing logbook and give AR No. to raw materials or intermediate.

·         AR No. Should be given as follows

  For Raw material: R-XXX/ZZ/R1 (e.g. R-001/08/R1)

  Where,   R          = raw material

                XXX    = serial no. (e.g. 001, 002, ….)

                ZZ        = year (e.g. 2008 as 08)

                R1        = re-test first time (e.g. R1, R2, ….)

               

·        Collect samples as per sampling plan.

·        After completion of sampling, do the necessary critical tests (e.g. assay, LOD, water content, pH, specific optical rotation etc.) as per the Standard Analytical Procedure.

·        Raw material may also be approved on the basis of physical appearance.

·        After completion testing, put the status of approved / rejected on the containers.

·        Re-testing of any raw materials should be four times only.

·        Frequency of re-testing for raw material is every year, and for intermediate is every six months. 

·        Re-testing should be performing on first come first out basis. The re-testing of material   should carry out, whose due date for re-test is earlier.  

6.0      Reference Document:

v     Re-testing of raw materials logbook.

     log book for Re-test raw material

S. No.	Date	Name of Raw material	Item code No.	Mfg. B. No.	Mfg. date	Exp. date

GRN No.	Manufacturer / Supplier	Re-test Due on	Sampled by	A.R. No. / Date	Withdraw by	Remarks
Format:-F/QC/012

Destruction of leftover / excess / rejected material

1.0              Purpose   :    To provide an instruction for destruction of leftover / excess / rejected material in QC department.

2.0               Objective   :     To provide a documented procedure for destruction of leftover / excess / rejected material in QC department.

3.0                   Scope     :    This procedure is applicable for destruction of leftover / excess / rejected material in QC department of --------Pharmaceuticals Ltd,Ankleshwar.

4.0         Responsibility   :

·       Primary  : QC Chemist / QC Officer

·       Secondary : Overall: QC – Incharge

5.0       Procedure:

·        Destruction of leftover/excess sample is carried out in QC washroom.

·        Bring the samples in area and remove and deface the label of materials.

·        Separate the waste in two parts Product (Raw materials, Powder, Liquids etc.) and Packing material (Labels, Jars, Foils, Cartons, Plastic bags, Glass Bottles, Caps, Tubes etc.)

·        Dissolve or suspend the product in bucket containing sufficient water, with the help of glass rod / hypo chlorite solution / acid / alkali or suitable reagents. 

·        If material soluble, neutralize and send it to ETP.

·        If not soluble, filter it and send residue for incineration.

·        Destroy the packing material waste separately in scrap yard.

Note: This procedure is applicable for leftover sample quantity after analysis, Expired control samples and Stability samples after testing.

Precautions:

Ø      Use acid / alkali proof hand gloves & safety goggles, safety shoes, nose mask.

Ø      Keep the exhaust/ventilation system ON.

Ø      Destruct the material by keeping the bucket away from the workman and material should be added slowly so that to avoid splashing.

Control Sample Handling

1.0         Purpose   :    To provide an instruction for control sample handling.

2.0         Objective  :   To provide a documented procedure for control sample handling.

3.0              Scope   :   This procedure is applicable for control sample handling in QC laboratory of ------  Pharmaceuticals Ltd,Ankleshwar.

4.0         Responsibility  :

·      Primary       : QC Chemist / QC Officer

·      Secondary   :  Overall: QC – Incharge 

5.0       Procedure    :

·      The samples drawn by the QC chemist shall be brought to Quality Control department.

·      Necessary entries shall be made in the Control Sample log book

·      After completion of testing and approved, prepare control sample for each products.

·      Quantity of control sample should be required two times testing (about 50 g).

·      Place the sample in white container and label to the box or to bottle to identify the     control samples under lock and key.

6.0      Reference Document   :

v           Control Sample logbook.

LOG BOOK FOR CONTROL SAMPLES

Product: __________             Product Code: __________               Year: _________

Sr No.	Date	Batch No.	Date of Mfg.	Date of Exp.	Qty	Analyzed by		Control sample		Due date for destruction	Remark
						Sign	Date	PartyName	Kept by
Format:-F/QC/011