ASTM E2503-2013e1 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践规程》.pdf

1、Designation: E2503 131Standard Practice forQualification of Basket and Paddle Dissolution Apparatus1This standard is issued under the fixed designation E2503; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio

2、n. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEEditorial corrections made throughout in April 2015.1. Scope1.1 This practice covers the set-up and calibration of thepaddle and basket d

3、issolution apparatus.1.2 Use of this practice may be applied 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 The values stated in SI units are to be regarded asstandard. No other units of measu

4、rement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limi

5、tations 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 results.2.2 Once a unit meets all of the mechanical specificationsincluded in this practice, it is considered calibrated

6、 and furthercalibration with dissolution calibrator tablets is not required.3. Analyst Responsibilities3.1 Verify the vessel, basket, and paddle dimensions onreceipt through measurement or Certificate of Analysis (COA)or Certificate of Conformity (COC).3.2 Ensure the instrument is calibrated and fit

7、 for perform-ing dissolution analysis.4. Procedure4.1 BackgroundThe set-up, mechanical, and operationalchecks are used to minimize variability during dissolutiontesting to ensure the reproducibility of dissolution results.4.2 Wherever possible, tools shall be traceable to an ac-cepted standard calib

8、ration source from a national or interna-tional calibration laboratory.4.3 Apparatus Set-upDuring apparatus installation or afterreplacement of parts or components, verify that the descriptionand critical dimensions for each part meets the originaldescription and dimension.4.3.1 Vessel DimensionsIn

9、the absence of a COA or COC,the vessels internal dimensions should be measured with anappropriate measuring device and vessel shape and conditionshould be noted. For example, for a cylindrical, hemisphericalvessel, the vessels sides must be cylindrical, the internaldimension should be measured, and

10、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 vessel.4.3.2 Basket/Shaft DimensionsIn the absence of a COA orCOC, an appropriate measuring device is used to measure therele

11、vant 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 thebasket-to-shaft adaptor, total basket height, internal diameter atthe top of the basket, outer diameter of the screen,

12、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 measuring device is used to measure therelevant dimensions of the paddle. Examples of dimensions tobe determined on each pa

13、ddle 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 top outer edge of the top of the blade, radiusof the outside edge of the blade, difference between thedistance from the mi

14、dline 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 manufacturers maintenancerecommendations and maintenance schedule to establish anappropriate maintenance program based on the freque

15、ncy ofapparatus use and quality system requirements.1This 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 Feb. 1, 2013. Published Ma

16、rch 2013. Originallyapproved in 2007. Last previous edition approved in 2007 as E2503 07. DOI:10.1520/E2503-13E01.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.5 Mechanical CalibrationPerform these tests on thefrequency determined

17、 by the quality system or after repair ormove. If the 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 equipm

18、ent, and these may be used. Depending onthe adjustments necessary to meet the mechanical calibrationcriteria, 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 touches the turning s

19、haft 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 runout.4.5.2 Paddle and

20、 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 within thelines of th

21、e 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 andminimum readings is the wob

22、ble. 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 shaft at two differentpos

23、itions: 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 to make it centered.

24、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 vesselmust not be more th

25、an 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-lated at two places 90 a

26、part.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 that the paddle/basket

27、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 stated rate, whichever isl

28、arger.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:4.6.1 Vessel ExaminationE

29、ach 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 deformed from itsoriginal c

30、onfiguration. 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 ofcoating sticking out fr

31、om 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 significant vibration

32、 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 apparatussmanufacturer, model number, and serial n

33、umber should berecorded on an appropriate Mechanical Calibration ReportSheet along with the appropriate observations. Calibrationreports need to include the results obtained originally and theresults after any adjustments or replacements are made. Ex-amples of report forms for apparatus that use six

34、 1-L vesselsthat are cylindrical with a hemispherical bottom, 165 mm highand 100 mm in diameter with paddle or basket 25 mm from thebottom are found in Appendix X1 and Appendix X2.6. Keywords6.1 basket dissolution apparatus; calibration; paddle disso-lution apparatusE2503 1312APPENDIXES(Nonmandatory

35、 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 1314