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Apr 30, 2011

SOP for Strip Packing Machine


1.0  OBJECTIVE:

       To lay down the procedure for Operation of Strip Packing Machine.

2.0  SCOPE:

       This SOP shall be applicable for the operation of Strip Packing Machine in Packing Area in Production department.

3.0  RESPONSIBILITY:

3.1  Execution               : Operator
3.2  Checking                : Production Pharmacist & Above

4.0  ACCOUNTABILITY:

       HOD-Production / Assigned Designee

5.0  PROCEDURE:

5.1  STRIP PACKING MACHINE OPERATION

5.1.1  Production person shall ensure the cleanliness of the Strip pack machine, its part & area and ‘CLEANED’ label on it.
5.1.2  Before starting the operation production person get the line clearance from Q.A person by writing the status label with Product Name, Batch Details to equipment & area.
5.1.3  Set up the strip-packing machine using appropriate change parts according to product.
5.1.4  Adjust the issued stereos on roller by double side adhesive tape.
5.1.5  Set the roller and back gear then set printed and plain ALU-ALU foil on roller.
5.1.6  Set the cutting gear, pinion gear and set vertical cutting manually or by adjusting the cutting gear.
5.1.7  Put “ON” the main switch, push button glowing in green color.
5.1.8  Put “ON” the heater & adjusts the temperature as per batch packing record.
5.1.9  Apply ink & thinner on the felt roller as and when required to get proper letter overprinting quality.
5.1.10  Start strip packing and collect specimen sample for checking of overprinting batch detail by operator / two production persons and Q.A person.
5.1.11  Attached the signed specimen to the BPR (batch packing record).
5.1.12  While the strip-pack machine is running, monitor on the indicator lamps of heater to ensure that the heaters are working satisfactorily as otherwise cooled down heater may result in bad sealing of strips. Record the actual temperature of sealing rollers in BPR. Record at specified intervals.
5.1.13  During the course of strip-packing at every half an hour to one hour interval Pharmacist should conduct random checks of the strips and counter check for:
•  Overprinted batch details on strips.                          
•  Sealing Quality.                       
•  Presence of any cut pockets/ Burst pocket.                          
•  No. of cuts per minute.        
•  Result of leak test.
5.1.14  Perform leak test on strips at specified intervals with specified No. of strips in Batch packing record or No. of strips in one sealing cycle.  Record the results in batch record.
5.1.15  After completion of operation, Put “OFF” the main supply.
5.1.16  Affix “To be Cleaned” status label and fill the “Equipment Log Book”.
NOTE:
•  Sufficient trial run should be taken to ensure satisfactory stripping before starting actual strip packing operation.
•  Written line clearance should be obtained from Q.A personnel before commencing strip packing and also prior to change over to another batch of same product or to a new product.
•  When strip packing is stopped during Tea/Lunch breaks, ensure that no tablets are left in the feed channel as otherwise tablets coming in contact with hot rollers may melt/get spoiled. When the machine is re-started, initially run some blank strips & ensure that proper overprinting of batch details from printing drum on plain foil is obtained, there after commence regular stripping of tablets.
During trial, strip should be collected from the machine. It should not send out to packing hall and de-foiled immediately.

6.0  ABBREVIATIONS:

6.1  SOP: Standard Operating Procedure
6.2  BMR: Batch Manufacturing Record
6.3  Q.A.: Quality Assurance
6.4  HOD: Head of The Department

Limit Test for Iron and Lead


Iron

Dissolve the specified quantity of the substance under examination in water, or prepare a solution as directed in the monograph, and transfer to a Nessler cylinder. Add 2 ml of a 20% w/v solution of iron-free citric acid and 0.1 ml of thioglycollic acid, mix, make alkaline with iron-free ammonia solution, dilute to 50 ml with water and allow standing for 5 minutes. Any color produced is not more intense than that obtained by treating in the same manner 2.0 ml of iron standard solution (20 ppm Fe) in place of the solution under examination.

Lead

The limit for lead is indicated in the individual monograph in terms of ppm, i.e., the parts of lead, Pb, per million parts (by weight) of the substance under examination.
The following method is based on the extraction of lead by solutions of dithizone.
All reagents used for the test should have as low a content of lead as practicable. All reagent solutions should be stored in containers of borosilicate glass. Glassware should be rinsed thoroughly with warm dilute nitric acid followed by water.

Method

Transfer the volume of the prepared sample directed in the monograph to a separator and, unless otherwise directed in monograph, add 6 ml of ammonium citrate solution and 2 ml of hydroxylamine hydrochloride solution. (For the determination of lead in iron salts use 10 ml of ammonium citrate solution). Add two drops of phenol red solution and make the solution just alkaline (red in color) by the addition of strong ammonia solution. Cool the solution if necessary and add 2 ml of potassium cyanide solution. Immediately extract the solution with several quantities, each of 5 ml, of dithizone extraction solution, draining off each extract into another separating funnel, until the dithizone extraction solution retains its green color. Shake the combined dithizone solution for 30 seconds with 30 ml of a 1 per cent v/v solution of nitric acid and discard the chloroform layer. Add to the acid solution exactly 5 ml of dithizone standard solution and shake for 30 seconds; the color of the chloroform layer is not more intense than that obtained by treating in the same manner a volume of lead standard solution (1ppm Pb) equivalent to the amount of lead permitted in the substance under examination, in place of the solution under examination.

Operation and Cleaning of Tray Dryer


Operation:

1.  Before operating the tray dryer, ensure that it is clean.
2.  Ensure that main switch is OFF.
3.  Load the material / accessories to be dried in the tray. Close the door of the tray dryer.
4.  Switch on the mains. Set the desired temperature as per BMR.
5.  Start the blower and then start the heater.

Cleaning:

1.  Switch OFF the electrical mains of tray dryer.
2.  Remove UNDER USE label and put TO BE CLEANED label.
3.  Remove the dust from the body with dry duster.
4.  Open the door. Remove all the trays and take it in washing area.
5.  Clean each tray by using potable water followed by 0.1% teepol solution using nylon scrubber.
6.  Clean each tray with 5 lit of potable water followed by 3 lit of purified water.
7.  Remove water with help of compressed air, dry all the trays with a clean dry lint free cloth.
Apr 29, 2011

SOP for Stirrer


1.0  OBJECTIVE:

       To lay down the procedure for Operation of Stirrer.

2.0  SCOPE:

       To lay down the procedure for Operation of Stirrer.

3.0  RESPONSIBILITY:

3.1  Execution              : Operator
3.2  Checking               : Production Pharmacist & Above

4.0  ACCOUNTABILITY:

       HOD-Production / Assigned Designee

5.0  PROCEDURE:

5.1  Production person shall ensure the cleanliness of the stirrer, its part & area and ‘CLEANED’ label on it.
5.2  Before starting the operation production person get the line clearance from Q.A person by writing the status label with Product Name, Batch Details to equipment & area.
5.3  Fix the shaft or propeller to the motor. Keep the shaft into the suspension to the half of the depth of suspension or up to that level so that suspension should not flush out.
5.4  Put “ON” the electric supply and start the stirring.
5.5  Stirring is carried out until uniform slurry is obtained or time specified in BMR.
5.6  Switch “OFF” the mains after completion of operation.
5.7  Affix “To be Cleaned" label. & fill the “Equipment Log Book”.

6.0  ABBREVIATIONS:

6.1  SOP: Standard Operating Procedure
6.2  BMR: Batch Manufacturing Record
6.3  Q.A.: Quality Assurance
6.4  HOD: Head of The Department

Pharmaceutical Administration and Regulations in Japan


Pharmaceutical Administration and Regulations in Japan
Front cover / Contents
CHAPTER 1. ORGANIZATION AND FUNCTION OF THE MINISTRY OF HEALTH, LABOUR AND WELFARE
CHAPTER 2. PHARMACEUTICAL LAWS AND REGULATIONS
CHAPTER 3. DRUG DEVELOPMENT
CHAPTER 4. POST-MARKETING SURVEILLANCE OF DRUGS
CHAPTER 5. SUPPLY AND DISSEMINATION OF DRUG INFORMATION
CHAPTER 6. HEALTH INSURANCE PROGRAMS AND DRUG PRICING IN JAPAN
Index
Apr 28, 2011

SOP for Colloid Mill


1.0  OBJECTIVE:

       To lay down the procedure for Operation of Colloid Mill.

2.0  SCOPE:

       This SOP shall be applicable for the operation of Colloid Mill in Coating area in Production department.

3.0  RESPONSIBILITY:

3.1  Execution              : Operator
3.2  Checking               : Production Pharmacist & Above

4.0  ACCOUNTABILITY:

       HOD-Production / Assigned Designee

5.0  PROCEDURE:

5.1  Production person shall ensure the cleanliness of the colloid mill, its part & area and ‘CLEANED’ label on it.
5.2  Before starting the operation production person get the line clearance from Q.A person by writing the status label with Product Name, Batch Details to equipment & area.
5.3  Fix the S.S. Rotor and stator at a necessary gap, to obtain a smooth slurry or suspension.
5.4  Fix the hopper, and if necessary circulating unit.
5.5  Put “ON” the mains.
5.6  Pass the slurry or suspension through colloid mill and check the consistency. If not smooth, re-pass through the colloid mill.
5.7  Put “OFF” the mains after completion of operation.
5.8  Affix “To be Cleaned” label and fill the “Equipment Log Book”.

6.0  ABBREVIATIONS:

6.1  SOP: Standard Operating Procedure
6.2  BMR: Batch Manufacturing Record
6.3  Q.A.: Quality Assurance
6.4  HOD: Head of The Department

Contents Uniformity (Weight or Volume) of Packaged Dosage Forms


The following tests and specifications apply to oral dosage forms and preparations intended for topical use that are packaged in containers in which the labeled net quantity is not more than 100 g or 300 ml or 1000 units, as the case may be. For higher labeled quantities the test and limits given in the standards of Weights and Measures (Packaged commodities) Rules, 1977 may be followed.

Ointments, Creams, Pastes, Granules and Powders for Oral Liquids.

Select a sample of 10 filled containers and remove any labeling that might be altered in weight while removing the contents of the containers. Clean and dry the outer surfaces of the containers and weigh each container. Remove quantitatively the contents from each container. If necessary, cut open the container and wash each empty container with a suitable solvent, taking care to ensure that the closure and other parts of the container are retained. Dry and again weigh each empty container together with its parts which may have been removed. The difference between the two weights is the net weight of the contents of the container.
The average net weight of the contents of the 10 containers is not less than the labeled amount and the net weight of the contents of any single containers is not less than 91 % and not more than 109 % of the labeled amount where the labeled amount is 50 g or less, or not less than 95.5 % and not more than 104.5 % of the labeled amount where the labeled is more than 50 g but not more than 100g.
If this requirement is not met, determine the net weight of the contents of 10 additional containers. The average net weight of the contents of the 20 containers is not less than the labeled amount, and the net weight of the contents of not more than 1 of the 20 containers is less than 91 % or more than 109 % of the labeled amount where the labeled amount is 50 g or less than 95 % or more than 104.5 % of the labeled amount is more than 50 g but not more than 100 g.

Liquids and suspensions

Viscous preparations- Select a sample of 10 filled containers and determine the weight of the contents of each container as directed under Ointments, Creams, Pastes, Granules and Powders for Oral Liquids. Determine the weight per ml and calculate the net volume of the contents of each container.
Non-viscous and free-flowing liquids- Pour completely the contents of each container into calibrated volume measures of the appropriate size and determine the volume of the contents of the 10 containers.
The average net volume of the contents of the 10 containers is not less than the labeled amount, and the net volume of the contents of any single containers is not less than 91 % and not more than 109 % of the labeled amount where the labeled amount is 50 ml or less, or not less than 95.5 % and not more than 104.5 % of the labeled amount where the labeled amount is more than 50 ml but not more than 200 ml, or not less than 97 % but not more than 103 % of the labeled amount where the labeled amount is more than 200 m1but not more than 300 ml, If this requirement is not met, determine the net volume of the contents of 10 additional containers. The average net volume of the contents of the 20 containers is not less than the labeled amount, and the net volume of the contents of not more than 1 of the 20 containers is less than 91 % or more than 109 % of the labeled amount where the labeled amount is 50 ml or less or less than 95.5 percent or more than 104.5 % of the labeled amount where the labeled amount is more than 50 ml but not more than 200 ml or less than 97 % or more than 103 % of the labeled amount where the labeled amount is more than 200 ml but not more than 300 ml.

Capsules, Pessaries, Suppositories and Tablets.

Select a sample of 10 containers and count the number of capsules, pessaries, suppositories or tablets in each container. The average number of the contents in the 10 containers is not less than the labeled amount and the number in any single container is not less than 98 % and not more than 102 % of the labeled amount. If this requirement is not met, count the number of the contents in 10 additional containers. The average number in the 20 containers is not less than the labeled amount, and the number in not more than 1 of the 20 containers is less than 98 % or more than 102 % of the labeled amount.

WHO News letter


WHO Newsletter on Risk Management Principles used for WHO Inspections of API facilities - 

Click here to view Newsletter

Operation and Cleaning of Tablet Inspection Machine


1.0  PRE START UP

1.1  Visually check the equipment and area for its cleanliness. Ensure that no remnant of previous product / batch is present.
1.2  Check the temperature and relative humidity of the area and record the details in the respective log books.
1.3  If the environmental conditions are not within the limit, do not start the operation and inform to the maintenance department.
1.4  If the conditions are within the limit start the operation.   
1.5  Ensure the status label on the machine.
1.6  Get the approval from In Process Quality Assurance Officer to start the operation.

2.0  OPERATION

2.1  Switch “ON” the main electric supply of the machine.
2.2  Check the machine for any abnormal noise by pushing the start switch button.
2.3  Place the tare polythene lined duly labeled high density polyethylene container below the discharge chute of machine for collection of inspected tablets.
2.4  Bring the trolley of tablets which is to be inspected near to the tablet inspection machine.
2.5  Feed the tablets to be inspected into the hopper of machine.
2.6  Set the vibration of vibrator as per the requirement.
2.7  Switch on the conveyor belt.
2.8  Check the tablets for any physical defects.
2.9  Collect the recoverable tablets from rejection box into a duly labeled high density polyethylene container.
2.10  When the high density polyethylene container gets filled at the discharge chute of machine replace it with another tare duly labeled high density polyethylene container.
2.11  Remove the container and tighten the bag with tie band and placed on separate trolley.

3.0  SHUT DOWN

3.1  After completion of operation switch OFF the machine.
3.2  Switch OFF the main electric supply of machine.
3.3  Transfer the tablets to the respective area.
3.4  Remove the status label from the machine and tear it off and put in the waste-bin.
3.5  Affix duly filled “TO BE CLEANED” Label on the equipment.

4.0  CLEANING

4.1  Remove the “TO BE CLEANED” Label from the equipment. Tear the label after checking the details on it.
4.2  Clean the hopper and conveyor belt using lint free cloth dipped in purified water.
4.3  Send rinse water sample intimation to IPQA.
4.4  Finally clean the machine using lint free cloth dipped in purified water followed by dry lint free cloth.
4.5  Clean the machine body with dry lint free cloth.
Apr 27, 2011

SOP for Volume Delivering Systems (Peristaltic Pump)


1.0  OBJECTIVE:

       To lay down the procedure for Operation of Volume Delivering Systems (Peristaltic Pump).

2.0  SCOPE:

       This SOP shall be applicable to Volume Delivering Systems (Peristaltic Pump) in Coating Area.

3.0  RESPONSIBILITY:

3.1  Execution              : Operator
3.2  Checking               : Production Pharmacist & Above

4.0  ACCOUNTABILITY:

       HOD-Production / Assigned Designee

5.0  PROCEDURE:

5.1  PERISTALTIC PUMP

5.1.1  Check the cleanliness of the Peristaltic Pump.
5.1.2  Switch “ON” the mains.
5.1.3  Check & set the Peristaltic Pump to required R.P.M. with adjusting knob.
5.1.4  Check for continuous flow of solvent.
5.1.5  After obtaining required R.P.M, check the volume of solution delivered with the help of calibrated measuring cylinder and starts compressed air to spray gun.
5.1.6  Check the spray and start coating as per the procedure.
5.1.7  Switch “OFF” the mains after completion of operation.
5.1.8  Affix “To Be Cleaned” Label and fill “Equipment Log Book”.

6.0  ABBREVIATIONS:

6.1  SOP  : Standard Operating Procedure
6.2  R.P.M : Revolution Per Minute
6.3  Q.A.   : Quality Assurance
6.4  HOD  : Head of The Department
Apr 26, 2011

SOP for Overprinting of Batch Details on Cartons and Catch Covers


1.0  OBJECTIVE:

       To lay down the procedure for overprinting of batch details on cartons and catch covers.

2.0  SCOPE:

       This SOP shall be applicable for all the batch overprinting operations carried out in Packing Department.

3.0  RESPONSIBILITY:

3.1  Execution              : Operator
3.2  Checking               : Production Pharmacist & Above

4.0  ACCOUNTABILITY:

       HOD-Production / Assigned Designee

5.0  PROCEDURE:

5.1  Production person shall ensure that, the printing area and printing machine are cleaned. Cartons / Catch covers of previous product are removed; stereos of previous product are removed and destroyed.
5.2  Before starting the operation production person get the line clearance from Q.A person by writing the status label with Product Name, batch Details to equipment & area and record the same in BMR.
5.3  Packing pharmacist should display the status label in front of overprinting machine and also give the instruction with batch details which is to be overprinted to the overprinting operator as per the BPR requirement.
5.4  Bring the cartons / catch covers issued for the batch to be overprinted, inside the printing area. Count the cartons / catch covers before starting the printing.
5.5  Obtain the overprinted rubber stereos required for the batch from Pharmacist and set the overprinted matter as per the instructions given by the Pharmacist.
5.6  First two overprinted cartons / catch covers should be signed and approved by:
               Overprinting Operator
               Two Packing Pharmacist
               Q.A. Person
5.7  Attach specimen samples to BPR (Batch Packing Record) and retain one sample in department for reference which should be destroyed after 3 months.
5.8  Before printing the sticked cartons should be separated and then taken for printing. The overprinted carton should be checked for any mixed up for unprinted carton.
5.9  Good overprinted cartons / catch covers should be collected and arranged in drum or cage trolley and should be labeled accordingly.
5.10  Quantity of printed cartons / catch covers and rejected quantity along with quantity of unprinted cartons, if any, should be recorded in the batch document as well as printing record.
5.11  Quantity of rejected cartons / catch covers recorded in a register and these cartons / catch covers should be destroyed by tearing into pieces in presence of Q.A. person followed by transfer into scrap yard for further destruction by burning/Shredding.
NOTE: If there should be any Break then, In case of Carton/catch cover the first Printed carton/ catch cover specimen should be checked & Signed by the Operator, Concerned Pharmacist & Q.A. Person. In case of Printed Foil, after the change of every Printed roll the Foil specimen to be attached in the respective BMR signed by Operator, Concerned Pharmacist & Q.A. Person.

6.0  ABBREVIATIONS:

6.1  SOP: Standard Operating Procedure
6.2  BMR: Batch Manufacturing Record
6.3  Q.A.: Quality Assurance
6.4  HOD: Head of The Department

Operation and Cleaning of Tablet Deduster Machine


PRE-START UP

1.  Ensure that no remains of previous product / batch is present.
2.  Visually check the equipment and area for its cleanliness.
3.  Affix “CLEANED” label on the equipment.
4.  Ensure specified temperature and relative humidity of the area.
5.  Ensure that the equipment is getting three phase alternating current supply.
6.  Ensure that the de-dusting machine is in working condition.
7.  Ensure that the operator is wearing proper gown, gloves and nose mask.
8.  Check the equipment usage log and ensure that equipment cleaning operation has been recorded.
9.  Take line clearance from QA and fill usage log.

OPERATION

1.  Replace “CLEANED” label with “UNDER PROCESS” label.
2.  Align tablet feeding mouth of de-dusting machine with tablet outlet chute of compression machine.
3.  Switch “ON” the equipment along with the compression machine.
4.  Collect de-dusted tablets in a double poly bag lined containers.
5.  Collect fine powder from powder collection box & treat it as recoverable.
6.  On completion of operation, switch “OFF” the equipment.
7.  Remove the dust collecting cup from the sifter chamber.
8.  Collect & weigh the dust.
9.  Record the weight in the relevant document.
10.  Replace “UNDER PROCESS” label with “TO BE CLEANED” label.

CLEANING

1.  Replace “UNDER PROCESS” label with “TO BE CLEANED” label.
2.  Remove loosely stuck powder from the machine by using vacuum cleaner duster and lint free cloth.
3.  Dismantle the machine in following sequence and keep the parts on pallet.
a.  Feed hopper
b.  Food grade gasket
c.  Perforated plate
d.  Dust collecting plate.
4.  Clean the dismantled sifting parts with the help of a nylon brush to remove any residual powder.
5.  Wash the equipment with raw water followed by 0.1% Teepol solution.
6.  Again wash with raw water to remove Teepol solution.
7.  Finally wash with purified water.
8.  Dry the parts using lint free cloth and inform the Q.A. department for collecting the rinse water sample.
9.  Clean the vibratory base mounting with a lint free wet cloth.
10.  Record the cleaning details in equipment log and sign it.

Precautions:-

(i)  Do not give sample from wet surface.
(ii)  Allow the water to run for five minutes before its use.
(iii)  Do not allow stagnant water at any place in equipment / container.
(iv)  Do not clean only the equipment desired for change over, all equipments in the same room will undergo cleaning in case of product change over.
Apr 25, 2011

SOP for Tablet Inspection Machine


1.0  OBJECTIVE:

       To lay down the procedure for Operation of Tablet Inspection Machine.

2.0  SCOPE:

       This SOP shall be applicable for operation of Tablet Inspection Machine in manufacturing area of Production department.

3.0  RESPONSIBILITY:

3.1  Execution               : Operator
3.2  Checking               : Production Pharmacist & Above

4.0  ACCOUNTABILITY:

       HOD-Production / Assigned Designee

5.0  PROCEDURE:

5.1  Check that the hoppers, feeder, trays and the conveyer belt along with the surrounding area for cleanliness.
5.2  Before starting the operation production person get the line clearance from Q.A person by writing the status label with Product Name, Batch Details to equipment & area.
5.3  Fix hopper, feeder & the trays in proper position and switch “ON” the electrical supply.
5.4  Start the belt & adjust its speed according to the convenience and Switch “ON” the tube lights.
5.5  Transfer tablets in the hopper and adjust the vibrator in such a way that a uniform and optimum flow of tablets is obtained.
5.6  Inspect the tablets for Appearance, Cracking, Broken Tablets, Lamination, Capping, Picking, Sticking, Mottling, Black Particles etc.
5.7  Collect all the rejected tablets separately in container labeled as rejected tablets. Weigh the tablets and mention its accountability in BMR.
5.8  Collect good tablets in clean double polythene bags contained in clean drums and label the product details on them.
5.9  Put “OFF” the mains, after operation is complete.
5.10  Affix “To Be Cleaned” label and fill the “Equipment Log Book”.

6.0  ABBREVIATIONS:

6.1  SOP: Standard Operating Procedure
6.2  BMR: Batch Manufacturing Record
6.3  Q.A.: Quality Assurance
6.4  HOD: Head of The Department

Thin-Layer Chromatography (TLC Method and Apparatus)


Thin-layer chromatography is a technique in which a solute undergoes distribution between two phases, a stationary phase acting through adsorption and a mobile phase in the form of a liquid. The adsorbent is a relatively thin, uniform layer of dry finely powdered material applied to a glass, plastic or metal sheet or plate. Glass plates are most commonly used. Separation may also be achieved on the basis of partition or a combination of partition and adsorption, depending on the particular type of support, its preparation and its use with different solvent.
Identification can be effected by observation of spots of identical Rf value and about equal magnitude obtained, respectively, with an unknown and a reference sample chromatographed on the same plate. A visual comparison of the size and intensity of the spots usually serves for semiquantitative estimation.

Apparatus

(a) Flat glass plates of appropriate dimensions which allow the application at specified points of the necessary quantities of the solution being examined and appropriate reference solutions and which allow accommodation of the specified migration path-length. The plates are prepared as described below; alternatively, commercially available pre-coated plates may be used.
(b) An aligning tray or a flat surface on which the plates can be aligned and rested when the coating substance is applied.
(c) The adsorbent or coating substance consisting of finely divided adsorbent materials, normally 5 micron to 40 micron in diameter, suitable for chromatography. It can be applied directly to the plate or can be bonded to the plate by means of Plaster of Paris (Hydrated Calcium Sulphate) or with any other suitable binders. The adsorbent may contain fluorescing material to help in visualising spots that absorb ultraviolet light.
(d) A spreader which, when moved over the glass plate, will apply a uniform layer of adsorbent of desired thickness over the entire surface of the plate.
(e) A storage rack to support the plates during drying and transportation.
(f) A developing chamber that can accommodate one or more plates and can be properly closed and sealed. The chamber is fitted with a plate support rack that supports the plates, back to back, with the lid of the chamber in place.
(g) Graduated micro-pipettes capable of delivering micro liter quantities say 10 ml and less.
(h) A reagent sprayer that will emit a fine spray and will not itself be attacked by the reagent.
(i) An ultraviolet light, suitable for observation at short (254 nm) and long (365 nm) ultraviolet wavelengths.

Related: Principle and Working of HPLC

Preparation of plates

Unless otherwise specified in the monograph, the plates are prepared in the following manner. Prepare a suspension of the coating substance in accordance with the instructions of the supplier and, using the spreading device designed for the purpose, spread a uniform layer of the suspension, 0.25 to 0.30 mm thick, on a flat glass plate 20 cm long. Allow the coated plates to dry in air, heat at 100° to 105° for at least 1 hour (except in the case of plates prepared with cellulose when heating for 10 minutes is normally sufficient) and allow to cool, protected from moisture. Store the plates protected from moisture and use within 3 days of preparation. At the time of use, dry the plates again, if necessary, as prescribed in the monograph.

Method

Unless unsaturated conditions are prescribed, prepare the tank by lining the walls with sheets of filter paper; pour into the tank, saturating the filter paper in the process, sufficient of the mobile phase to form a layer of solvent 5 to 10mm deep, close the tank and allow standing for 1hour at room temperature. Remove a narrow strip of the coating substance, about 5 mm wide, from the vertical sides of the plate. Apply the solutions being examined in the form of circular spots about 2 to 6 mm in diameter, or in the form of bands (10 to 20 mm x 2 to 6 mm unless otherwise specified) on a line parallel with, and 20 mm from, one end of the plate, and not nearer than 20 mm to the sides; the spots should be 15 mm apart. If necessary, the solutions may be applied in portions, drying between applications. Mark the sides of the plate 15 cm, or the distance specified in the monograph, from the starting line. Allow the solvent to evaporate and place the plate in the tank, ensuring that it is as nearly vertical as possible and that the spots or bands are above the level of the mobile phase. Close the tank and allow standing at room temperature, until the mobile phase has ascended to the marked line. Remove the plate and dry it.
For two-dimensional chromatography dry the plate after the first development and carry out the second development in a direction perpendicular to the first.
When the method prescribed in the monograph specifies 'protected from light' or 'in subdued light' it is intended that the entire procedure is carried out under these conditions.

Adjustment of chromatographic conditions

Minor adjustments to the parameters of the test may be made in order to satisfy the system suitability criteria. These may be:
Mobile phase. Minor solvent component of a mixture: ± 30 per cent relative or ± 2 per cent absolute, whichever is the larger; no other component altered by more than 10 per cent absolute;
Concentration of salts. In the buffer component of the mobile phase; ± 10 per cent; pH of the aqueous component of the mobile phase. ± 0.2 pH, unless otherwise stated in the monograph, or ± 0.1 pH, when neutral substances are to be examined;
Volume of solutions applied: 10-20 per cent of the prescribed volume if plates have fine particles (2-10 micron).

Visualisation

After development, the plate should be examined under an ultraviolet light having a maximum output at about 254 nm or at about 365 nm, as the case may be. Alternatively, it may be visualised as directed in the monograph; where a spraying technique is prescribed it is essential that the reagent be evenly applied as a fine spray. The term secondary spot means any spot other than the principal spot. Similarly, a secondary band is any band other than the principal band.

Semi-quantitative estimation

Identification. The principal spot in the chromatogram obtained with the test solution is visually compared to the corresponding spot in the chromatogram obtained with the reference solution in respect of the color, the size and the Rf of the spots.
Test for Related substances. The secondary spot(s) in the chromatogram obtained with the test solution is (are) visually compared to either the corresponding spot(s) in the chromatogram obtained with the reference solution containing the impurity (ies) or the spot in the chromatogram obtained with the reference solution prepared from a dilution of the test solution.

Quantitative measurement

The substances that have been separated after development of the plate and that respond to UV-Vis irradiation can be estimated directly on the plate with suitable instrumentation. Measurement is of the reflectance of the incident light from the spots by moving the plate or the measuring device. Likewise, fluorescence may be measured using an appropriate optical system.

Apparatus

The apparatus for direct measurement consist of: a device for exact positioning and reproducible application of the amount of solutions onto the plate, a mechanical device for moving the plate or the measuring device along the x-axis or the y-axis, a recorder and a suitable integrator or a computer, and a photometer with a source of light, an optical device for generating monochromatic light and a photo cell of adequate sensitivity; for measurement of fluorescence, a suitable filter to prevent light used for excitation from reaching the detector while permitting emitted light or a specific portion thereof to pass.

Method

Prepare the test solution and reference solutions as prescribed in the individual monograph. Use the same solvent for all the solutions and apply the same volume of each and develop the plate. Prepare and apply not fewer than 3 reference solutions of the substance under examination, the concentrations of which span the expected value in the test solution (about 80 per cent, 100 per cent and 120 per cent).
Treat with the prescribed reagent, if necessary, and record the reflectance, the transmittance or fluorescence in the chromatograms obtained with all the solutions. Use the measured results to calculate the amount of substance in the test solution. The requirement for resolution and separation are prescribed in the individual monograph.
Apr 24, 2011

SOP for Vacuum Cleaner


1.0  OBJECTIVE:

       To lay down a procedure for operating and cleaning of Vacuum Cleaner.

2.0  SCOPE:

       This SOP shall be applicable for operation and cleaning of Vacuum Cleaner in production area.

3.0  RESPONSIBILITY:

3.1  Execution              : Operator
3.2  Checking               : Production Pharmacist & Above

4.0  ACCOUNTABILITY:

       HOD-Production / Assigned Designee

5.0  PROCEDURE:

5.1  OPERATING

5.1.1  Connect the top with power supply and put "ON" the switch. Use flexible hosepipe along with accessories as per requirement to collect the dust from respective area for Batch to Batch cleaning. Switch "OFF" the vacuum cleaner after use. Use dedicated vacuum cleaner for respective area.

5.2  CLEANING PROCEDURE OF VACUUM CLEANER FREQUENCY:

At the end of the day or whenever required.
5.2.1  Transfer the vacuum cleaner and accessories to the respective wash area having status label 'To be cleaned'.

5.2.2  HOSE PIPE CLEANING

5.2.2.1  Detach hose pipe from vacuum cleaner and socking probe. Flush the inner & outer surface of the hose pipe with potable water.
5.2.2.2  Drain the water & allow it to dry.
5.2.2.3  Wipe the outer surface with clean dry lint free cloth.
5.2.2.4  Cover the hose pipe with polythene cover.

5.2.3  BODY CLEANING

5.2.3.1  Remove the filter bag and tap it in a polythene bag to remove dust.
5.2.3.2  If dust remains in filter bag, use disposable nylon scrubber to remove the dust from filter bag.
5.2.3.3  Collect the dust in waste bin. Wash the filter bag with potable water. Allow the filter bag to dry.
5.2.3.4  Wipe the collection tank with cleaned dry lint free cloth.
5.2.3.5  Fit the clean dry filter bag and Hose pipe to the vacuum cleaner.
5.2.3.6  Cover the end of hose pipe with polythene bags.
5.3  Affix the status label 'Cleaned' with signature & date.
5.4  Transfer the cleaned Vacuum Cleaner to respective area.

6.0  ABBREVIATIONS:

6.1  SOP: Standard Operating Procedure
6.2  Q.A.: Quality Assurance
6.3  HOD: Head of The Department

Operation and Cleaning of Roll Compector


PRE-STARTUP

1.  Check the cleanliness of the room.
2.  Check the material lying in the room and ensure that it is of the same batch to proceed.
3.  Remove the clean tag of the equipment and tear them off after confirming the details.
4.  Put the equipment label on the machine.
5.  Check the room temperature and relative humidity and record it in BMR / environment control monitoring card if it is not within the limit inform the maintenance department and do not proceed till it gets rectified.

STARTUP:

Operation:

1.  Check and ensure the cleanliness of the machine.
2.  Bring the material near to the equipment, to be compacted.
3.  Switch ON the main power supply.
4.  Check and ensure the switch position in forward direction for starting the compaction on the operation panel board.
5.  Turn ON the main switch from the operation panel board.
6.  Press the green push button to start the roller.
7.  Press the green push button to start the auger.
8.  Set the speed of the roller and auger in RPM as per product specification mentioned in BMR.
9.  Record the equipment operation details in the equipment log card.
10.  Charge the feed hopper with materials to be compacted using cleaned scoops.
11.  Record the equipment operation details in the equipment log card.

Shutdown:

1.  Switch OFF the machine by pressing the key panel of the machine.
2.  Inform the maintenance people to switch OFF main power supply from electrical panel board on the service floor.

CLEANING

1.  Remove loosely stucked power from the machine by using vacuum cleaner, duster and lint free cloth.
2.  Dismantle the machine in the following sequence and keep parts on pallet.
a.  SS covering plate
b.  Charging hopper
c.  Discharge chute.
3.  Clean the exterior of the machine by vacuum cleaner and lint free cloth.
4.  Wash the dismantled parts with running water followed by rinsing with purified water.
5.  Wipe all part with 2% NaOH solution using cotton duster and allow it to remain as such for 5 to 10 minutes.
6.  Clean all above parts in running potable water using cotton duster.
7.  Rinse all above parts with sufficient quantity of purified water.
8.  Collect the final rinse in properly identified conical flask and send the same to Q.A. department.
9.  Dry the dismantled parts using dryer.
10.  Assemble the cleaned dismantled parts.
11.  After cleaning affix the cleaned equipment tag on the equipment.
12.  Record the cleaning details in the equipment log card.
Apr 23, 2011

SOP for Deburring & Dedusting Machine


1.0  OBJECTIVE:

       To lay down the procedure for Operation of De-burring & De-dusting Machine.

2.0  SCOPE:

       This SOP shall be applicable for the operation of De-burring & De-dusting Machine in Compression area in Production department.

3.0  RESPONSIBILITY:

3.1  Execution              : Operator
3.2  Checking               : Production Pharmacist & Above

4.0  ACCOUNTABILITY:

       HOD-Production / Assigned Designee

5.0  PROCEDURE:

5.1  ROTARY TABLET DE-DUSTER

5.1.1  Production person shall ensure the cleanliness of the De-burring and de-dusting machine and ‘CLEANED’ label on it.
5.1.2  Before starting the operation production person get the line clearance from Q.A person by writing the status label with Product Name, Batch Details to equipment.
5.1.3  Fix the receiving chute and S.S. body to the motor assembly.
5.1.4  Fix the connecting hose pipe of receiving chute and S.S. body with compression machine.
5.1.5  Put “ON” electric supply & start the machine for dedusting operation.
5.1.6  Start Compression Machine.
5.1.7  Put the trays at the end of shift or after completion of the batch under compression and destroys the fines obtained by soaking in water.
5.1.8  Affix “To Be Cleaned” label after operation is complete.
5.1.9  Fill “Equipment Log Book”.

6.0  ABBREVIATIONS:

6.1  SOP: Standard Operating Procedure
6.2  BMR: Batch Manufacturing Record
6.3  Q.A.: Quality Assurance
6.4  HOD: Head of The Department