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Automated analysis by yatin sankharva   copy Automated analysis by yatin sankharva copy Presentation Transcript

  • Prepared By: Mr. PARTH P. M. Pharm, Sem –II Q. A. Department-SJTPC Guided By: Mr. Jignesh S. ShahAsst. Professor of Q. A. Department-SJTPC, Rajkot 1
  • Contents Benefits of Automation Need for Automation Objective of Automation Classification of Automatic analyzers Types of Automatic analysis technique Automation approach in analysis Basic Automatic Analysis System Automated Method in P’Copoeia Good Automated Laboratory Practices 2
  • . “One machine can do the work of fifty ordinary men, no machine can do the work of one extraordinary man” Complete automation will lead to human prohibition in pharma industries. 3
  • DefinitionIUPAC define automation as ‘the use of combinations of mechanical and instrumental devices to replace, refine, extend or supplement human effort and facilities in the performance of a given process, in which at least one major operation is controlled without human intervention, by a feedback mechanism’.Mechanization, on the other hand, is defined as ‘the use of mechanical devices to replace, refine, extend or supplement human effort’. The distinction between the two terms is quite clear according to IUPAC ,insofar as ‘automation’ describes systems that involve a feedback loop 4
  • Human Accuracy & precision Cost cutting prohibitionToo large number of sample Increasing number of analyte Advance automation in microchip , and Complex statistical calculation Strict regulation microprocessor5
  • Benefits of AutomationFaster analyses up to 120 samples per hourUp to 300 samples can be analyzed in batchAutomatic data recording and preparationBeing a closed system, automation reduces contamination, for e.g., from atmospheric gasesGreater accuracy and reproducibility of results as all samples are subject to same processesSmaller sample and reagent volumes which reduces costAutomatic range changing, drift control and automatic sample preparation 6
  • Need for automation. The partial or complete replacement of human participation in laboratory process is a growing trend Increasingly stricter control of growing number of samples in which a large number of analyts are to be determined at increasingly low concentration Cost reduction In research for increased accuracy, precision, and productivity, the pharmaceutical analyst seeks to select optimal measurement and to automate as appropriate 7
  • Automated device They are defined as those encasing automation. They are conceived to make decisions with the aid of feedback system, without human intervention. There is a different operation sequence for each situation (sample).Some system are self-monitoring and self-adjusting ,have greater independence than automatic devices and are sometimes called ‘completely automatic’. 8
  • Objective of Automation Automation is used for:-  Facilitating an analytical technique or method  Processing of large number of samples  Determination of several components in the same sample  Reduction of human participation to  Avoid error  Cut costs  Increasing sample throughput  Process (industrial or otherwise ) control  Lowering consumption of sample and/or reagent(s)  Samples, occasionally dealt with in large number or valuable to deal with manually  Analyts, which are sometime present in very dissimilar or low concentration in sample. 9
  • .Reagents, some of which are rare or expensive even unstable.Rapidity, frequently essential in large laboratories such as those in hospitals, urgently requiring the analytical result, and of industrial and other laboratories require in constant availability of data for process controls.Economy, in personnel and material expenditure.Precision, closely related to the elimination of both definite and indefinite errors arising from the so-called ‘human factor’ (tiredness, mood, prejudice, pathological, complaints and so forth)Data generation , some analytical technique are based on the acquisition of a large number do data, especially in the drug discovery and development stages. 10
  • Classification of automatic analyzers:  According to the degree of automation  Automatic  semi-automatic  According to the way in which samples and reagents are transported  Batch (discrete)  Continuous  Segmented  Unsegmented  Robotics  According to the number of analytes per sample  One parameter  Multi-parameter 11
  •  According to flexibility  Specific  Flexible According to source  Commercial  Hand-made According to the state of aggregation of sample  Gas analyzer  Liquid analyzer  Solid analyzer According to sample frequency  One-off  Periodic  Continuous 12
  • Types of Automatic Analysis Technique  Basically there are two types of automatic analysis techniques/instruments:-Discrete sampling instrument- In discrete sampling, each sample undergoes reaction and measurement in a separate cuvet or chamber. These samples may be analyzed sequentially or in parallel.Continuous –flow sampling instrument- In continuous flow sampling, the samples flow sequentially and continuously in tube perhaps being separated by air bubble. They are each sequentially mixed with reagent in the same tube at the sample point down stream and then flow sequentially into a detector 13
  • A. Continuous Flow AnalysisThere are two kind of Continuous Flow Analysis:i. Segmented flow analysisIt includes a peristaltic pump that continuously aspirates sample and reagent, a variable no. of tubes constituting a manifold to circulate liquid and a detector system.Aspirated sample are segmented by injecting air bubbles that should be remove before they can be reaching to the detector.At detector air bubble are removed and thus each sample is separated by washing solution, thus a square shaped detector response is obtained, the height of rectangle is directly proportional to conc. of analyte. 14
  • .ii. Flow Injection Analysis FIA is like a HPLC without a column. It is low pressure and without separation. The injected sample mixes and reacts with the flowing stream. A transient signal is recorded. FIA is based on the injection of a liquid sample into a moving continuous nonsegmented carrier stream of a suitable liquid. The injected sample forms a zone which is then transported towards a detector. Mixing with reagent in the flowing stream mainly occurs by diffusion-controlled process and a chemical reaction occurs. Detectors continuously record the physical parameter as it changes as a result of passage of sample material through flow cell. 15
  •                                                                                               Flow Injection Analysis Flow Injection Analysis 16
  • .There are mainly five types Flow Injection Analysis: i. Syringe based injection system ii. Injection with rotary valve iii. Proportional injection iv. Merged injection v. Hydrodynamic injectionComparison of peaks of SFA and FIA SFA peak FIA peak 17
  • B. Discrete Analyzers ( Batch Analyzer)A discrete analyzer handles each individual sample as a separate entity and is usually a single channel instrument.In some designs both sample and reagent are metered into discrete reaction vessels.However , most of the system have specially design cells that already contain pre pack amount of required reagent for given analyte and thus making sample introduction only the necessary step.In both cases reagents are combine with sample in discrete cuvettes where mixing, incubation and final color measurement occurs. 18
  • Automation Approach in Analysis: 1. A serial (or sequential ) automation process 2. A parallel automation process 3. Hybrid Automation Systems 19
  • 1.A Serial (Sequential) Automation Process The general characteristic of a serial automation process is that a given determination reaches completion before the next determination begins, although with some serial automation systems, the second determination may be started before the first is completed. Serial automation could also be configured in an on-line arrangement, where tandem processes in the chemical determination are performed by collection from a flowing stream. 20
  • 2.Parallel Automation Process Parallel Automation Process  for chemical analysis is, simply, a process where more than one automated chemical manipulation is performed simultaneously. These parallel manipulations can encompass some or all of the following discrete analytical chemistry operations:  Experiment initiation,  Sampling (obtaining the samples),  Sample preparation,  Component separation,  Analyts detection and  reduction/reporting   21
  •  Such an on-line system could be used to  acquire a sample,  process it, and  perform the associated chemical measurement step E.g.. in the case of  on- line micro dialysis/LC/MS or  on-line solid-phase extraction/LC/MS/MS 22
  • 3. Hybrid Automation SystemsHybrid automation systems for chemical analysis combine features of both serial and parallel systems.Some processes are conducted in serial, some are conducted in parallel, and all are integrated into a single system Tomtec Quadra-96 liquid handling workstation. Conceptualized semi automated 96-well liquid–liquid extraction procedure. Zymark combinatorial chemistry workstation 23
  • Hybrid Automation = Serial Automation + Parallel Automation.Hybrid Automation Systems  In Robotic solid-phase extraction method development system, a central robotic arm (XP) which service various arm peripherals, and a 144-port vacuum manifold, used for solid-phase extraction method development.  The system and development of the solid-phase extraction columns, which are in parallel. Although a fully parallel system would have been desirable, it was beyond the capabilities of commercially available system at this time. 24
  • Basic Automatic Analysis System Sampling unit Proportioning pump Manifolds Dialyzers Constant temperature bath Detector Recorder 25
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  • Sampling unit: The sampling unit enables an operator to introduce unmeasured sample and standards into auto analysis system. The unit in its earlier form consisted of a circular turntable. The sample plate carrying these cups rotates at a predetermined speed. The movement of turntable is synchronized with the movements of sampling crook. The crook carries a thin flexible polythene tube, which can dip into cup and allow water, standard or test solution to be aspirated. The samplers are fitted with a sample mixer, which enables the sample to be mixed before and during aspiration. The automatic samplers employs a different washing action between samples. 27
  • Proportioning Pump:. The function of proportioning pump is to continuously and simultaneously push the fluids, air and gases through the analytical chain. Samples and reagents are driven single peristaltic pump. A series of flexible plastic tubes, one from the sampler the other from reagent bottles or simply drawing air, are placed length wise along the platen spring loaded platform. The roller head assembly is driven by a constant speed gear motor. When the rollers are pressed down and the motor switched on, they compress the tube containing liquid streams against the platen. As the roller advance across the platen, they drive the liquid before them. 28
  • Manifolds: A manifold mainly consists of a platter, pump tubes, coils, transmission tubing, fittings and connections. Mixing coils are used to mix the sample/reagent. As the mixture through a coil, the air bubble along with the rise and fall moton produces a completely homogenous mixture. Delay coils are employed when a specimen must be delayed for a completion of chemical reaction before reaching the colorimeter. Various types of fittings are employed to join stream of liquids to split a stream or to introduce a air segmentation to the stream. The reagents line are segmented by introducing air through one or more additional tubes in the manifold. This produces a series of bubbles at a regular intervals in the liquid stream. This is designated as bubble pattern 29
  • Dialyzer:. Dialysis is accomplished to remove protein cells to obtain an interference free analysis. The dialyzer module consists of a pair of Perspex plates, the mating surface of which are mirror grooved in a continuous channel, which goes in towards the centre on itself and returns to the outside. A semi permeable cellophane membrane is clamped between the two plates. Cellophane membrane use has a pore size of 40-60Å. 30
  • Constant temperature bath:On leaving the dialyzer, the stream may be combined by one or more additional reagents. It is then passed to a heating bath. A thermostatically controlled immersion heater maintains a constant temperature within ±0.1.Detector system:- Mainly used detector Colorimeter Flame photo meter FlourimeterSignal Processing and Data-Handling:Modern automatic analysis systems make use of a PC as multi tasking data processor and system controller. However such multi tasking is used with the use of microprocessor based analogue interface card which fits neatly into a standard extension slot inside the computer. 31
  • Recorder:. The most common type of recorder used with automated system is dc voltage null-balance potentiometer recorder. Significant fluctuations in the flow pattern may result in irregularities of the base line on a recorder. Irregularities are also produced due to a drift in the electronic circuit. Pulse suppressor are used to smoothen out fluctuations. 32
  • Automated Method in P’CopoeiaAutomated method have been found especially useful in testing the content uniformity of tablets and capsules and in facilitating methods requiring precisely controlled experimental conditions.In addition,the detection system and calculation of results for automated methods are often computerized.Before, an automated method for testing an article is adopted as an alternative, it is advisable to ascertain that the results obtained by this system are equivalent in accuracy and precision to those obtained by the prescribed p’copoeial method.Because of their versatility, this system designed for rapid determination of specified substance often can be readily modified by the addition of suitable modules and accessories to permit the determination of one or more additional substance in dosage form.e.g.in the automated analysis of articles containing both estrogen & progestogens. 33
  • Good Automated Laboratory Practices The foundation of GALP standards comprises six principles inherent in the EPA’s GLP requirements and its data management policies.1. The system must provide a method of assuring the integrity of all entered data.2. The formulas and decision algorithms employed by the system must be accurate and appropriate.3. An audit trail must track data entry and modification to the responsible individual.4. A consistent and appropriate change control procedure must be capable of tracking the system operation and application software.5. Appropriate user procedure must be followed.6. Alternative plans for the system failure, disaster recovery and unauthorized access must be developed. 34
  • FEATURES AND ADVANTAGES OF AUTOMATION SYSTEMS Speed. Complexity. Hardware.  Redundancy of hardware Software. Expandability. Unattended operation. Error recovery. 35
  • SummaryDue to the ongoing demand for speed in industrial chemical analysis, parallel automation processes are beginning to replace serial automation processes, especially in those areas where high numbers of assays or samples are expected.For in situ or on-line situations where sparse strategic sampling is the norm, serial automation will likely play a continued role.Expensive robotic arms, while powerful and flexible, do not directly lend themselves to parallel automation systems unless the effort is made to combine them with specialized multichannel hardware. Such hybrid systems are powerful and useful but are extremely complicated to implement and maintain.In the future, it seems likely that automated systems will be miniaturized and that this miniaturized format will lend itself readily to increased use of automation. 36
  • Reference Norbert R,Kuzel,Harold E,Roudebush & Charles E.S, (1969),”Automation techniques in pharmaceutical analysis”,Journal of pharmaceutical sciences,vol.58,no.4,381- 406. Edward H.Kerns,Li DI,(2005) “Automation in pharmaceutical profiling” ,Chemical and Screening Science, Wyeth Research,Princeton,NJ,114-123. Berridge J.C,(1990), “Advance in automation of pharmaceutical analysis”, Analytical chemistry department, Pfizer central research,vol.7,No.12.pp.1313-1321. David G.C, Thoru Sugawara, “Laboratory Automation in Chemical Industries”,Marcel Dekker Sugawara,T.,Cork,D.G.LaboratoryRoboticsandAutomation8:2 21–230,1996. Skoog, D. A., West, D. M., and Holler, F. J. Fundamentals of Analytical Chemistry, 7th ed., Saunders College Publishing, 37 Philadelphia, 1996.
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