ASTM E2503-2007 Standard Practice for Qualification of Basket and Paddle Dissolution Apparatus《篮式和搅拌溶解器具合格的标准实施规范》.pdf

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1、Designation: E 2503 07Standard Practice forQualification of Basket and Paddle Dissolution Apparatus1This standard is issued under the fixed designation E 2503; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi

2、on. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers the set-up and calibration of thepaddle and basket dissolution apparatus.1.2 Use of this practice may be ap

3、plied to apparatus thathave been modified to enable automatic dissolution testing(that is, a valve in the bottom of the vessel or sampling throughthe shaft).1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user o

4、f this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Significance and Use2.1 This practice outlines a procedure for the mechanicalcalibration of paddle and basket dissolution units to ensurereproducibility of

5、 results.2.2 Once a unit meets all of the mechanical specificationsincluded in this practice, it is considered calibrated and furthercalibration with dissolution calibrator tablets is not required.3. Analyst Responsibilities3.1 Verify the vessel, basket, and paddle dimensions onreceipt through measu

6、rement or Certificate of Analysis (COA)or Certificate of Conformity (COC).3.2 Ensure the instrument is calibrated and fit for perform-ing dissolution analysis.4. Procedure4.1 BackgroundThe set-up, mechanical, and operationalchecks are used to minimize variability during dissolutiontesting to ensure

7、the reproducibility of dissolution results.4.2 Wherever possible, tools shall be traceable to an ac-cepted standard calibration source from a national or interna-tional calibration laboratory.4.3 Apparatus Set-upDuring apparatus installation or af-ter replacement of parts or components, verify that

8、the descrip-tion and critical dimensions for each part meets the originaldescription and dimension.4.3.1 Vessel DimensionsIn the absence of a COAor COC,the vessels internal dimensions should be measured with anappropriate measuring device and vessel shape and conditionshould be noted. For example, f

9、or a cylindrical, hemisphericalvessel, the vessels sides must be cylindrical, the internaldimension should be measured, and the vessel bottom shouldbe smooth and without defects. The vessel must fit within theapparatus in such a manner as to ensure stable operation andcentering of the shaft in the v

10、essel.4.3.2 Basket/Shaft DimensionsIn the absence of a COAorCOC, an appropriate measuring device is used to measure therelevant basket dimensions. Critical dimensions to be mea-sured on each basket should include but are not limited to: shaftdiameter, vent hole diameter, thickness of wide portion of

11、 thebasket-to-shaft adaptor, total basket height, internal diameter atthe top of the basket, outer diameter of the screen, height of theopen screen, outer diameter of bottom, diameter of screen onthe bottom, and screen mesh number.4.3.3 Paddle DimensionsIn the absence of a COA orCOC, an appropriate

12、measuring device is used to measure therelevant dimensions of the paddle. Examples of dimensions tobe determined on each paddle should include but are notlimited to: shaft diameter, blade height, blade thickness, totalblade length, length of flat portion on bottom of blade, radiusof the angle on the

13、 top outer edge of the top of the blade, radiusof the outside edge of the blade, difference between thedistance from the midline of the shaft to the top outer edge forthe two sides, and difference between the heights of both sidesof the paddles at the outside top.4.4 MaintenanceConsult the manufactu

14、rers maintenancerecommendations and maintenance schedule to establish anappropriate maintenance program based on the frequency ofapparatus use and quality system requirements.4.5 Mechanical CalibrationPerform these tests on thefrequency determined by the quality system or after repair ormove. If the

15、 instrument is not in routine use, the mechanicalcalibration may be performed before performing the firstdissolution test. Some instrument manufacturers supply specialtools or incorporate automatic mechanical calibration deviceswithin their equipment, and these may be used. Depending onthe adjustmen

16、ts necessary to meet the mechanical calibration1This practice is under the jurisdiction of ASTM Committee E55 on Manufac-ture of Pharmaceutical Products and is the direct responsibility of SubcommitteeE55.03 on General Pharmaceutical Standards.Current edition approved March 15, 2007. Published April

17、 2007.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.criteria, the position and orientation of each vessel may need tobe noted to ensure proper subsequent set-up.4.5.1 Shaft WobbleA runout gauge is positioned so thatthe gauge probe

18、touches the turning shaft about 2 cm above thetop of the paddle blade or basket. The gauge is placed so thatthe probe slightly presses in on the turning shaft. The absolutevalue of the difference between the maximum and minimumreadings is the wobble. The measured value must not exceed1.0 mm total ru

19、nout.4.5.2 Paddle and Basket Shaft VerticalityUse an accuratebubble level or digital leveling device to determine that theshafts are vertical in two directions 90 apart around thevertical axis while the drive unit is in the operating position. Ifa bubble level is used, the bubble should be centered

20、within thelines of the level. If necessary, the verticality may be checkedwith the shafts raised above the drive unit.4.5.3 Basket WobbleA runout gauge is positioned so thatthe gauge probe touches the bottom rim of the turning basket.The absolute value of the difference between the maximum andminimu

21、m readings is the wobble. The measured value must notexceed 1.0 mm total runout.4.5.4 Vessel CenteringA mechanical or digital centeringdevice that measures centering inside the vessel is required.The centering device is used to center the vessels around thepaddle or basket shafts or a surrogate shaf

22、t at two differentpositions: at the top rim of the vessel and above the bottomportion of the vessel just above the basket or paddle position.Slowly turn the shaft and check the centering at both levels. Ifthe vessel is not centered on either level, adjust the vessel permanufacturers recommendations

23、to make it centered. Repeatthis process until both bottom and top positions are centeredwithin 1 mm from the center line.4.5.5 Vessel VerticalityAfter raising the apparatus head, aleveling device can then be placed on the inside wall of thevessel. Measure the vessel at two points, 90 apart. The vess

24、elmust not be more than 1.0 from vertical at either position.Alternatively, calculations can be done to determine vesselverticality using information from a centering device (twomeasurements taken directly above each other at a knownheight apart for each calculation.) Verticality should be calcu-lat

25、ed at two places 90 apart.4.5.6 Basket and Paddle DepthIf the height of the paddle/basket is adjustable, a depth gauge is used to set the distancebetween the bottom of each of the paddle blades or baskets andthe bottom of the vessels. An adjustable depth gauge or otherdevice can be used to verify th

26、at the paddle/basket height iswithin 8 % of desired height. For example, for a paddle at 25mm from the bottom, the height needs to be 62 mm.4.5.7 Rotational SpeedA tachometer is used to measurethe rotational speed of the paddle or basket. The rate of rotationmust be within 2 % or 62 rpm of the state

27、d rate, whichever islarger.4.5.8 Vessels Temperature SensorIf the system has athermal sensor in each vessel to check the temperature of themedium, the performance of each thermal sensor should beverified against a traceable standard.4.6 OperationBefore each dissolution test perform thefollowing:4.6.

28、1 Vessel ExaminationEach vessel must be free ofscratches, cracks, pits, and residue.4.6.2 Basket ExaminationEach basket must be free ofdefects such as rusting or corrosion, any wires sticking outbeyond the basket, clogged mesh holes, and dented mesh sidesor bottom. Make sure the basket is not deform

29、ed from itsoriginal configuration. Verify that the method of attaching thebasket to the shaft (that is, clips, O-rings, and so forth) is theone described in the analytical method to be used.4.6.3 Paddle ExaminationEach paddle must be visuallyexamined for defects such as rusting and loose pieces ofco

30、ating sticking out from the paddles (for paddles coated withpolytetrafluoroethylene (PTFE) or another coating).4.6.4 Vessel TemperatureThe temperature of the mediuminside each vessel is measured at time of use. The mediumtemperature must be 60.5C from the target value.4.6.5 VibrationThere can be no

31、significant vibration in thedissolution apparatus or medium. Possible sources of vibrationare the surrounding environment, the dissolution unit itself orone of its components or an external water bath circulatingheater.5. Report5.1 The date, analyst, and the dissolution apparatuss manu-facturer, mod

32、el number, and serial number should be recordedon an appropriate Mechanical Calibration Report Sheet alongwith the appropriate observations. Calibration reports need toinclude the results obtained originally and the results after anyadjustments or replacements are made. Examples of reportforms for a

33、pparatus that use six 1-L vessels that are cylindricalwith a hemispherical bottom, 165 mm high and 100 mm indiameter with paddle or basket 25 mm from the bottom arefound in Appendix X1 and Appendix X2.6. Keywords6.1 basket dissolution apparatus; calibration; paddle disso-lution apparatusE2503072APPE

34、NDIXES(Nonmandatory Information)X1. BASKET APPARATUS QUALIFICATION REPORT SHEETDate _ Analyst _Dissolution Apparatus: Manufacturer _ Model #_ Serial #_ Dissolution Vessels: Manufacturer _MECHANICAL CALIBRATION REPORT SHEETBASKET APPARATUSCalibrationParameterPoint ofMeasurementResults or through the ASTM website(www.astm.org).E2503074