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![ASSAY EXAMPLES:
1. Assay of paracetamol tablets was done using HPLC and the following results
were obtained
Data
Weight of 20 tablets=12.2243 g
Weight of tablet powder taken for assay=152.5 mg
Stated content per tablet=500 mg
Original volume=200 ml
Dilution steps
• 20 ml into 100 ml
• 10 ml into 100 ml
• Calibration curve for paracetamol: Y= 35656X + 80 where X is in mg/100 ml
• Area of peak obtained for paracetamol in diluted sample extract =44 519
I. Calculate the percentage of stated content in paracetamol tablets
II. Does the product pass the QC test for assay? [BP limit: 95%-105%]](https://image.slidesharecdn.com/02goodlaboratorypracticeglp1-220912174713-dfb4540c/85/02Good-Laboratory-Practice-GLP-1-pptx-25-320.jpg)
![2. Assay of methyl dopa tablets was done as follow [BP, 2007].
10 tablets of methyl dopa were weighed and powdered. The quantity of powder
equivalent to 0.25 gm of methyl dopa was taken and dissolved in 0.05 M H2SO4 to
produce 100 ml and filtered using filter paper. 5 ml of the filtrate was taken and 2
ml of iron (II) sulphate –citrate solution and sufficient water was added to produce
100 ml. The absorbance of the resulting solution was measured at 550 nm and
the following results were obtained.
Stated content of methyl dopa per tablet=250 mg
Weight of 10 tablets=4.5 g
Absorbance reading of sample solution at 550 nm =0.425
Absorbance reading of standard solution(12.5 mg/100 ml) at 550 nm =0.445
a. Calculate the percentage of the stated amount of methyl dopa in the tablets
b.Does the product pass the Qc test for assay? [BP limit: 95%-105%]](https://image.slidesharecdn.com/02goodlaboratorypracticeglp1-220912174713-dfb4540c/85/02Good-Laboratory-Practice-GLP-1-pptx-26-320.jpg)
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02Good Laboratory Practice (GLP)(1).pptx
- 1. GOOD LABORATORY PRACTICE(GLP) GLP is one of the components of QA Concerned with the activities of QC laboratories carrying out tests & assay methods required to establish the compliance of the product with specification claimed for them. Main goal is to help laboratories obtain results which are reliable, repeatable and recognized worldwide 1
- 2. GOOD LABORATORY PRACTICE… The quality of the product is achieved through GMP & monitored with GLP guide line The guide line provide guidance to the laboratory control of pharmaceutical products performed either in: The manufacturing firm Regulatory laboratories Research laboratories Objectives of GLP makes sure that the data submitted are a true reflection of the results that are obtained during the study makes sure that data is traceable Promotes international acceptance of tests 2
- 3. BASIC ELEMENTS OFGLP 1. Personnel Should have appropriate qualification, experience and training in QC Availability of protective clothing and other safety facilities Availability of periodic training program for all personnel Sufficient people 2. Facilities: Include laboratory building, furniture, etc The laboratory should have suitable size, construction & location to facilitate the proper condition of the test 3
- 4. BASIC ELEMENTS OFGLP 2.1 Design & construction guide line Locate in area free from noise, vibration, etc to prevent interference QC lab should be designed of sufficient space: to suit the analytical operation to be performed to avoid mix-up and cross contamination etc. QC lab should have adequate storage for sample to be analyzed Physico-chemical and microbiological laboratories etc. should be separated each other
- 5. BASIC ELEMENTS OFGLP … 3. Equipments: 3.1 Equipment design Equipments shall be appropriate design and suitably located for operation, cleaning & maintenance Major instruments of a testing laboratory Analytical balance, IR , UV-Visible, GC, pH meter, dissolution & disintegration test apparatus, potentiometer, KFT, HPLC, flame photometer, AAS, HPTLC Equipment for microbiological laboratory Autoclave, microscope, incubators, centrifuge with refrigerator, membrane filters 5
- 6. BASIC ELEMENT OFGLP … 3.2. Maintenance & calibration Availability of qualified & experienced personnel Detailed SOPs which describe: the instrument, calibration standards & limits, calibration for each instruments, record keeping requirements etc. Preventive maintenance: Is very important for assuring that the instrument is in good operating condition
- 7. BASIC ELEMENT OFGLP … 4. Testing operation SOPs Are written documents specifying the procedure that must be followed to carry out the operations Benefits: Prevents introduction of errors & variations by avoiding word of mouth communication or reliance on memory Used to train personnel & thus help to prevent misunderstanding Eliminate need to develop the procedure every time an operation is performed etc 7
- 8. BASIC ELEMENTS OFGLP … Chemical, reagent & solutions Storage should follow the storage conditions recommended on the label Highly toxic chemicals should be stored in appropriate place Solution & reagents to be prepared in the laboratory should follow the procedure in the pharmacopeia & label properly Requirements: Reagents and solutions shall be labeled Deteriorated or outdated reagents and solutions shall not be used Include Date opened Stored under ambient temperature Expiration date 8
- 9. REFERENCE STANDARDS The accuracyand precision of test results and test methods is dependant on the reliability, authenticity and control over reference standards, reagents and stock solutions Similarly the retrospective testing of materials and product is dependant on the protection and storage of retention samples Primary Standards may be obtained from National reference labs In House Secondary Standards Standardized against primary standards using definitive methods 9
- 10. BASIC ELEMENT OFGLP … 5. Test articles: Drug testing laboratories receive d/t type of samples for test and control among which are: finished pharmaceutical products APIs Dressing, suturing materials Medical devices 10
- 11. BASIC ELEMENTS OFGLP … 6. Record & reports Records: Records regarding the d/t test applied & all readings and calculation should be maintained in a bound laboratory book Record of the preparation of solution & reagents, standardization of solutions, raw data etc Type of documents Standard operating procedures , Protocols of tests, results & Reports 11
- 12. Laboratory records Laboratory recordsshall include complete data derived from all tests necessary to assure compliance with established specifications and standards Description and identification of sample received Description of method of testing Record of all data secured in the course of the test Record of test results and how they compare with standards of identity, strength and quality Record of all deviations and modification of test Record of standardization of reference standards Record of calibration of equipments 12
- 13. BASIC ELEMENT OFGLP … Reporting of results It is a GLP requirement that a final report should be reported for each analytical work completed E.g. tablets & capsule Name of the sample Date of receipt of the sample Analytical report No Batch/lot No Protocol of the test applied – description, identification, weight uniformity, disintegration time, result of assay Signature of analyst Opinion & signature of the approved analyst Signature of the laboratory head 13
- 14. QUALITY CONTROL (QC) Qualitycontrol: is a term that refers to processes involved in maintaining the quality and validity of a manufactured product Each holder of a manufacturing authorization should have a quality control department QC department should be independent from other department The QC department must have adequate resource Adequate laboratory facilities or access to them Appropriately qualified, trained and experienced personnel Approved written procedures 14
- 15. THE OPERATIONAL TASKOF THE QUALITY CONTROL DEPARTMENT: Sampling Inspecting Analytical testing- to confirm compliance with specification Releasing or rejecting material for production use and finished products useful in monitoring product quality during storage/ distribution/ use Approve/reject drug products made by other company Approve or reject all procedures or specifications affecting drug product 15
- 16. SCOPE OF QC Itemsconcerned : Starting materials Packaging materials Intermediates Bulk products Finished products 16
- 17. QC Responsibilities: 1. Testingof bulk components prior to use by production and finished product prior to release for sale 2. Release product, based on QC test results 3. Approval of suppliers: selection of suppliers who can supply starting and packaging materials Testing of representative samples is required to ensure compliance with GMP requirements 4. In process QC (IPQC) 5. Sampling: All sampling should be representative of the batch and that it is done in accordance with an SOP
- 18. QC RESPONSIBILITIES: 6. Adequaterecords: Records must be kept of all sampling, inspecting and testing of raw materials and finished products. This is a key part of traceability 7. Sample retention To allow evaluation of the product after it has gone on sale if there is a need Finished product: kept for 1 year past the expiry date Starting materials: Kept for 2 years after the date of release of the finished product
- 19. QC RESPONSIBILITIES: 8. Evaluationof complaints: Evaluation of all complaints received and taking appropriate actions accordingly Sometimes, complaints may necessitate a product recall decision 9. Product recall: The QC department is responsible for the product recall decision and examination of the returned products to determine whether such products should be released, reprocessed or destroyed
- 20. BASIC REQUIREMENTS FORQUALITY CONTROL: 1. Sampling should be under taken by methods and personnel approved by the QC department It must be carried out in such a way that it is representative of the batch and in accordance with an SOP QC personnel must have access to the production area to undertake sampling when necessary. 2. Records for sampling, testing of materials, intermediates and bulk and finished products need to be kept This means that there will be traceability on what happened. 20
- 21. BASIC REQUIREMENTS FORQUALITY CONTROL … 3. Validated test methods should be applied Test methods should be challenged to be able to demonstrate that the tests are able to give an accurate result on repeatable bases The method must be capable of being applied with precision The results obtained must be linear over a range of acceptable response the result must be repeatable over a number of identical tests The validation of test methods includes: Accuracy, Precision, Linearity, Repeatability, Robustness and Specificity
- 22. BASIC REQUIREMENTS FORQUALITY CONTROL … 4. The QC department should review and evaluate relevant production documentation This review need to cover all quality aspects - to assure no errors have occurred Ensures manufacturing documentations and the QA documentation are in harmony 5. The QC department should generate or review records for deviations and failure investigations it is important that all deviation from the normal manufacturing procedure are recorded or documented Any impact on product quality must be assessed 22
- 23. BASIC REQUIREMENTS FORQUALITY CONTROL … 6. QC ensures that ingredients used comply with the qualitative and quantitative composition of the finished product as approved in market authorization 7. QC ensure that proper containers are used 8. QC ensures correct labeling of finished products 9. QC ensures batches are released by appropriate authorization 23
- 24. BASIC REQUIREMENTS FORQUALITY CONTROL … 10. Sample of starting materials & finished products are retained. Sufficient retention samples of the starting materials and the finished products in its final pack should be kept for one year past the expire date. This is to allow for an evaluation of the product after it has been distributed should there be a need. It will also allow ongoing stability trial to be done 24
- 25. ASSAY EXAMPLES: 1. Assayof paracetamol tablets was done using HPLC and the following results were obtained Data Weight of 20 tablets=12.2243 g Weight of tablet powder taken for assay=152.5 mg Stated content per tablet=500 mg Original volume=200 ml Dilution steps • 20 ml into 100 ml • 10 ml into 100 ml • Calibration curve for paracetamol: Y= 35656X + 80 where X is in mg/100 ml • Area of peak obtained for paracetamol in diluted sample extract =44 519 I. Calculate the percentage of stated content in paracetamol tablets II. Does the product pass the QC test for assay? [BP limit: 95%-105%]
- 26. 2. Assay ofmethyl dopa tablets was done as follow [BP, 2007]. 10 tablets of methyl dopa were weighed and powdered. The quantity of powder equivalent to 0.25 gm of methyl dopa was taken and dissolved in 0.05 M H2SO4 to produce 100 ml and filtered using filter paper. 5 ml of the filtrate was taken and 2 ml of iron (II) sulphate –citrate solution and sufficient water was added to produce 100 ml. The absorbance of the resulting solution was measured at 550 nm and the following results were obtained. Stated content of methyl dopa per tablet=250 mg Weight of 10 tablets=4.5 g Absorbance reading of sample solution at 550 nm =0.425 Absorbance reading of standard solution(12.5 mg/100 ml) at 550 nm =0.445 a. Calculate the percentage of the stated amount of methyl dopa in the tablets b.Does the product pass the Qc test for assay? [BP limit: 95%-105%]
Editor's Notes
- #13 Laboratory records shall include complete data derived from all tests necessary to assure compliance with established specifications and standards, including examinations and assays, as follows: A description of the sample received for testing with identification of source (that is, location from where sample was obtained), quantity, lot number, date sample was taken, and date sample was received for testing. A statement of each method used in the testing of the sample. The suitability of all testing methods used shall be verified under actual conditions of use. A complete record of all data secured in the course of each test, including all graphs, charts, and spectra from laboratory instrumentation, properly identified to show the lot tested. A record of all calculations performed in connection with the test, including units of measure, conversion factors etc. Results of tests and how the results compare with established standards of identity, strength, quality, and purity. The initials or signature of the person who performs each test and the date(s) the tests were performed. The initials or signature of a second person showing review for accuracy, completeness, and compliance Complete records shall be maintained of any modification of an established method employed in testing. Complete records shall be maintained of any testing and standardization of laboratory reference standards, reagents, and standard solutions. Complete records shall be maintained of the periodic calibration of laboratory instruments and recording devices
- #15 Quality Control is a process employed to ensure a certain level of quality in a product or service. To a pharmaceutical manufacturer it implies a detailed system of inspection and control covering the evaluation, production and distribution of every drug, with the objectives to produce medications of superior efficacy and safety and to provide assurance to the physician, the pharmacist and the consumer that a given product performs uniformly and in a satisfactory manner for the purpose for which it is recommended. The pharmaceutical quality control laboratory serves one of the most important functions in pharmaceutical evaluation, production and distribution .
- #16 Some of the responsibilities of QC areas follows : Approve or reject all components, drug product containers, in-process materials, packaging material, labeling and drug products. Authority to review production records to assure no errors have occurred, or if have occurred, have been fully investigated. Approve/reject drug products made by other company. Must have adequate lab facilities for testing/approval/rejection of components, drug product containers, in-process materials, packaging material, labeling and drug products. Approve or reject all procedures or specificationsaffecting drug product. Responsibilities/procedures must be in writing and must be followed.