ASTM E2503-2013 Standard Practice for Qualification of Basket and Paddle Dissolution Apparatus《筐和桨溶解装置合格标准的标准实施规程》.pdf

1、Designation: E2503 07E2503 13Standard 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

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

3、 be applied to apparatus that have been modified to enable automatic dissolution testing (that is,a valve in the bottom of the vessel or sampling through the shaft).1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This

4、standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Significance and Use2.1

5、 This practice outlines a procedure for the mechanical calibration of paddle and basket dissolution units to ensurereproducibility of results.2.2 Once a unit meets all of the mechanical specifications included in this practice, it is considered calibrated and furthercalibration with dissolution cali

6、brator tablets is not required.3. Analyst Responsibilities3.1 Verify the vessel, basket, and paddle dimensions on receipt through measurement or Certificate of Analysis (COA) orCertificate of Conformity (COC).3.2 Ensure the instrument is calibrated and fit for performing dissolution analysis.4. Proc

7、edure4.1 BackgroundThe set-up, mechanical, and operational checks are used to minimize variability during dissolution testing toensure the reproducibility of dissolution results.4.2 Wherever possible, tools shall be traceable to an accepted standard calibration source from a national or internationa

8、lcalibration laboratory.4.3 Apparatus Set-upDuring apparatus installation or after replacement of parts or components, verify that the description andcritical dimensions for each part meets the original description and dimension.4.3.1 Vessel DimensionsIn the absence of a COA or COC, the vessels inte

9、rnal dimensions should be measured with anappropriate measuring device and vessel shape and condition should be noted. For example, for a cylindrical, hemispherical vessel,the vessels sides must be cylindrical, the internal dimension should be measured, and the vessel bottom should be smooth andwith

10、out defects. The vessel must fit within the apparatus in such a manner as to ensure stable operation and centering of the shaftin the vessel.4.3.2 Basket/Shaft DimensionsIn the absence of a COA or COC, an appropriate measuring device is used to measure therelevant basket dimensions. Critical dimensi

11、ons to be measured on each basket should include but are not limited to: shaft diameter,vent hole diameter, thickness of wide portion of the basket-to-shaft adaptor, total basket height, internal diameter at the top of thebasket, outer diameter of the screen, height of the open screen, outer diamete

12、r of bottom, diameter of screen on the bottom, andscreen mesh number.1 This practice is under the jurisdiction of ASTM Committee E55 on Manufacture of Pharmaceutical Products and is the direct responsibility of Subcommittee E55.03 onGeneral Pharmaceutical Standards.Current edition approved March 15,

13、 2007Feb. 1, 2013. Published April 2007 March 2013. Originally approved in 2007. Last previous edition approved in 2007 as E2503 07. DOI: 10.1520/E2503-07.10.1520/E2503-13.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes

14、 have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official

15、 document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.3.3 Paddle DimensionsIn the absence of a COA or COC, an appropriate measuring device is used to measure the relevantdimensions of the paddle. Examples of dimensions to be det

16、ermined on each paddle should include but are not limited to: shaftdiameter, blade height, blade thickness, total blade length, length of flat portion on bottom of blade, radius of the angle on the topouter edge of the top of the blade, radius of the outside edge of the blade, difference between the

17、 distance from the midline of theshaft to the top outer edge for the two sides, and difference between the heights of both sides of the paddles at the outside top.4.4 MaintenanceConsult the manufacturers maintenance recommendations and maintenance schedule to establish anappropriate maintenance prog

18、ram based on the frequency of apparatus use and quality system requirements.4.5 Mechanical CalibrationPerform these tests on the frequency determined by the quality system or after repair or move.If the instrument is not in routine use, the mechanical calibration may be performed before performing t

19、he first dissolution test.Some instrument manufacturers supply special tools or incorporate automatic mechanical calibration devices within theirequipment, and these may be used. Depending on the adjustments necessary to meet the mechanical calibration criteria, theposition and orientation of each v

20、essel may need to be noted to ensure proper subsequent set-up.4.5.1 Shaft WobbleA runout gauge is positioned so that the gauge probe touches the turning shaft about 2 cm above the topof the paddle blade or basket. The gauge is placed so that the probe slightly presses in on the turning shaft. The ab

21、solute valueof the difference between the maximum and minimum readings is the wobble. The measured value must not exceed 1.0 mm totalrunout.4.5.2 Paddle and Basket Shaft VerticalityUse an accurate bubble level or digital leveling device to determine that the shaftsare vertical in two directions 90 a

22、part around the vertical axis while the drive unit is in the operating position. If a bubble levelis used, the bubble should be centered within the lines of the level. If necessary, the verticality may be checked with the shaftsraised above the drive unit.4.5.3 Basket WobbleA runout gauge is positio

23、ned so that the gauge probe touches the bottom rim of the turning basket. Theabsolute value of the difference between the maximum and minimum readings is the wobble. The measured value must not exceed1.0 mm total runout.4.5.4 Vessel CenteringA mechanical or digital centering device that measures cen

24、tering inside the vessel is required. Thecentering device is used to center the vessels around the paddle or basket shafts or a surrogate shaft at two different positions: atthe top rim of the vessel and above the bottom portion of the vessel just above the basket or paddle position. Slowly turn the

25、 shaftand check the centering at both levels. If the vessel is not centered on either level, adjust the vessel per manufacturersrecommendations to make it centered. Repeat this process until both bottom and top positions are centered within 1 mm from thecenter line.4.5.5 Vessel VerticalityAfter rais

26、ing the apparatus head, a leveling device can then be placed on the inside wall of the vessel.Measure the vessel at two points, 90 apart. The vessel must not be more than 1.0 from vertical at either position. Alternatively,calculations can be done to determine vessel verticality using information fr

27、om a centering device (two measurements takendirectly above each other at a known height apart for each calculation.) Verticality should be calculated 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 distancebetwee

28、n the bottom of each of the paddle blades or baskets and the bottom of the vessels.An adjustable depth gauge or other devicecan be used to verify that the paddle/basket height is within 8 % of desired height. For example, for a paddle at 25 mm from thebottom, the height needs to be 62 mm.4.5.7 Rotat

29、ional SpeedAtachometer is used to measure the rotational speed of the paddle or basket. The rate of rotation mustbe within 2 % or 62 rpm of the stated rate, whichever is larger.4.5.8 Vessels Temperature SensorIf the system has a thermal sensor in each vessel to check the temperature of the medium,th

30、e performance of each thermal sensor should be verified against a traceable standard.4.6 OperationBefore each dissolution test perform the following:4.6.1 Vessel ExaminationEach vessel must be free of scratches, cracks, pits, and residue.4.6.2 Basket ExaminationEach basket must be free of defects su

31、ch as rusting or corrosion, any wires sticking out beyond thebasket, clogged mesh holes, and dented mesh sides or bottom. Make sure the basket is not deformed from its original configuration.Verify that the method of attaching the basket to the shaft (that is, clips, O-rings, and so forth) is the on

32、e described in the analyticalmethod to be used.4.6.3 Paddle ExaminationEach paddle must be visually examined for defects such as rusting and loose pieces of coatingsticking out from the paddles (for paddles coated with polytetrafluoroethylene (PTFE) or another coating).4.6.4 Vessel TemperatureThe te

33、mperature of the medium inside 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 in the dissolution apparatus or medium. Possible sources of vibration arethe surrounding environment, the dissolution

34、unit itself or one of its components or an external water bath circulating heater.5. Report5.1 The date, analyst, and the dissolution apparatuss manufacturer, model number, and serial number should be recorded onan appropriate Mechanical Calibration Report Sheet along with the appropriate observatio

35、ns. Calibration reports need to includeE2503 132the results obtained originally and the results after any adjustments or replacements are made. Examples of report forms forapparatus that use six 1-L vessels that are cylindrical with a hemispherical bottom, 165 mm high and 100 mm in diameter withpadd

36、le or basket 25 mm from the bottom are found in Appendix X1 and Appendix X2.6. Keywords6.1 basket dissolution apparatus; calibration; paddle dissolution apparatusAPPENDIXES(Nonmandatory Information)X1. BASKET APPARATUS QUALIFICATION REPORT SHEETDate _ Analyst _Dissolution Apparatus: Manufacturer _ M

37、odel #_ Serial #_ Dissolution Vessels: Manufacturer _MECHANICAL CALIBRATION REPORT SHEETBASKET APPARATUSCalibrationParameterPoint ofMeasurement Results or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).E2503 135