USP泼尼松校正片说明书(中英文对照)(共8页).docx

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1、精选优质文档-倾情为你奉上Certificate（证书）PREDNISONE TABLETS（泼尼松片）USP Catalog No.: USP Lot No.: R031Y1(10 mg nominal prednisone content per tablet) （每片含泼尼松10mg）FOR DISSOLUTION PERFORMANCE VERIFICATION TEST (PVT) 用于溶出性能确认实验Period of validity: This certificate of USP Prednisone Tablets Lot R031Y1 is valid through J

2、une 30th, 2017.有效期：USP泼尼松片批号R031Y1的证书有效期到2017年6月30日The USP Prednisone Tablets RS is provided for use in the Performance Verification Test for USP Apparatus 1 and 2 with 1 liter vessels in the USP General Test Chapter on DISSOLUTION and DRUG RELEASE , APPARATUS SUITABILITY. Store in a dry place. Stor

3、e the tablets at controlled room temperature not exceeding 25.USP泼尼松标准片用于采取USP中方法1和方法2对1升溶出杯，进行USP通用测试部分溶出（711）和释放（724）项目的性能能确认实验，药品贮藏在干燥，温度低于25环境中。Dissolution Medium: We recommend preparing the medium as follows:Heat a suitable amount of water, while stirring gently, to about 41-45. Filter under va

4、cuum through a 0.45-m-porosity filter into a suitable filtering flask equipped with a stirring device. Seal the flask and continue to apply vacuum while stirring for an additional five minutes. Measured vacuum should be less than 100 mbar. The temperature of the Dissolution medium should not fall be

5、low 37 prior to the initiation of the test.溶出介质：推荐介质准备（操作）如下：（脱气纯化水）加热适量水同时轻轻搅拌到约4145。真空下用0.45m滤膜过滤至配有搅拌容器中（即过滤后需要搅拌），密封容器口并继续在真空条件下搅拌5分钟。检测真空度小于100 mbar。在实验开始前溶出介质温度不高于37。Procedure：See DISSOLUTION in the current USP: Determine the quantity of prednisone, C21H26O5, dissolvedat 30 minutes, in each ve

6、ssel, expressed as percent of the labeled amount. Use 499 g of Dissolution Medium (which corresponds to 500 mL), where possible the medium should not be stirred prior to the initiation of the test for the purpose of equilibration, and conduct the test at 37. Operate each apparatus at 50- rpm speed.

7、Withdraw an aliquot of sample solution at 30 minutes and filter immediately. Measure the amount of prednisone dissolved from filtered portions of the sample aliquots at 242 nm in comparison with a solution of known concentration of USP Prednisone Reference Standard.步骤：查看USP现行版的溶出711：确定泼尼松数量，每个溶出杯中溶解

8、30分钟，结果用百分比表示。499g溶出介质（相当于500ml溶出介质），为了达到溶出介质平衡，实验开始前不能搅拌溶出介质并且温度控制37。开启转速50转。30分钟时取样马上过滤。在242nm波长下测定溶出度（百分比表示）与已知浓度的USP泼尼松参考标准比较。实验条件：500ml溶出介质、37、50转/分钟、30分钟取样检测： 242nm的波长下测定供试品溶液和对照品溶液的溶出度Note: An amount of alcohol not to exceed 5% of the total volume of the standard solution may be used to bring

9、 the prednisone reference standard into solution.The filtering method must not cause absorptive loss of drug.Bras introduced by automated methods is to be avoided.If equipment is dedicated for use with only one apparatus (basket or paddie).then performance verification is only required for that appa

10、ratus.At the time of use ,peel back the paper-backed lidding to remove the tablets from the blister card注意：1、 乙醇的用量应不超过总体积的 1。（对照品先用少量乙醇溶解以加快溶解速度）；2、 自动取样系统可以减少偏差；3、如果只仪器只用一种方法（转篮或桨板），仅仅需要对使用的方法进行确认；est Interpretation: Laboratory can choose either of the test schemes listed below.实验说明：从以下实验方案中选择一种Si

11、ngle-Stage Test单阶实验：The following are step-by-step instructions for the Single-Stage test.单阶实验操作步骤：1. For each position in the assembly, test one USP Prednisone Tablets RS, and record the percent dissolved at the sampling time point specified. Transform the percent dissolved results to the natural l

12、og scale, determine the mean and variance. For assemblies with 12 or 14 positions (12 or 14 dissolution vessels), no further testing is required.1.每个溶出杯中放入一粒USP泼尼松片，按照选取方法在规定时间点取样并检测溶出度。先将各个溶出度数据计算得到自然对数，再以自然对数为数据，计算其平均数（X1）和方差（1）,12个和14个溶出杯的仪器可以不再进行后续检测。2. For assemblies with fewer than 12 position

13、s, repeat Step 1 with an additional set of tablets. Again after transforming the percent dissolved results to the natural log scale, determine the mean and variance.2. 不到12个溶出杯的仪器，重复第1步操作，即再次向每个溶出杯中放入一粒USP泼尼松片，按照选取方法在规定时间点取样并检测溶出度。将检测得到的各个溶出杯结果计算平均数（X2）和方差（2）3. Calculate the average of the two means

14、 and of the two variances obtained in Steps 1 and 2. (Use the results from Step 1 alone for assemblies that have 12 or 14 positions.)3将第1、2步中得到的两个平均值（X1、X2）和方差（1、2）分别计算各自的平均值。即X3=X1+X22，3=1+22，（12个或者14个溶出杯无需计算，直接取用第1步计算结果，即X3=X1，3=1）4. Convert the results of Step 3 to a geometric mean (GM) and perce

15、nt coefficient of variation (%CV). See calculation example below for more detail.4.第3步中计算得到的X3和3按照以下公式计算得到GM和%CV。GM=eX3%CV=100e3-15. Compare the results of Step 4 to the Single-Stage acceptance ranges in Table 1. The GM must not fall outside the limits,and the %CV must not be greater than the limit.

16、 If both meet the criteria, the assembly has passed the PVT.5.第4步计算得到的GM和%CV结果与表格1中“Single-Stage”项下的相应标准比较。GM不能低于范围下限；%CV需要高于限度标准。如果两个结果均符合标准，性能确认通过。Microsoft Excel中对应的各个计算公式：自然对数：LNX：AVERAGE：VAR.SeX: EXPX: SQRTOptional Two-Stage Test：双阶实验A laboratory may choose to implement the PVT as a Two-Stage t

17、est in case of assemblies with less than 12 positions. The Two-Stage test is a statistically valid means of allowing the possibility of stopping the test at the first stage with a penalty. The following are step-by-step instructions for the two-stage test. 出杯数量小于12个的情况下，实验室可以选择双阶实验作为性能确认。双阶实验是一个有效统计

18、方法允许第一阶段（the first stage）实验结果不合格情况下进行后续第二阶段实验（the second stage）。操作步骤如下。1. For each position in the assembly, test one USP Prednisone Tablets RS, and record the percent dissolved at the sampling time point specified. After transforming the percent dissolved results to the natural log scale, determine

19、 the mean and variance.1.每个溶出杯中放入一粒USP泼尼松片，按照选取方法在规定时间点取样并检测溶出度。先将各个溶出度数据计算得到自然对数，再以自然对数为数据，计算其平均数（X1）和方差（1）。2. Convert the results of Step 1 to a GM and %CV, and compare to the 1st Stage of Two Stages acceptance ranges in Table 1. The GM must not fall outside the limits, and the %CV must not be gre

20、ater than the limit. For calculation of the GM and %CV, see calculation example for more detail. 2. 第1步中计算得到的X3和3按照以下公式计算得到GM和%CV。并与表格1中“1st Stage of Two Stages”项下的相应标准比较。GM不能低于范围下限；%CV需要高于限度标准。GM=eX1%CV=100e1-13. If results of Step 2 satisfy both acceptance criteria, the assembly has passed the PVT

21、. Otherwise continue to Step 4. (see note 1).3. 如果第2步两个结果均符合标准，性能确认通过，否则需要继续第4步操（见备注1）。4. Repeat Step 1 with an additional set of tablets and after transforming the percent dissolved results to the natural log scale determine the mean and variance for the data obtained at this step.4. 向每个溶出杯中放入一粒USP

22、泼尼松片，按照选取方法在规定时间点取样并检测溶出度。将检测得到的各个溶出杯结果计算平均数（X2）和方差（2）5. Average the two means and two variances obtained in Steps 1and 4. 将第1步和第4步双阶实验得到的平均值和方差计算得平均数两个平均值（X1、X2）和方差（1、2）分别计算各自的平均值。即X3=X1+X22，3=1+22， 6. Convert the results of Step 5 to a geometric mean (GM) and percent coefficient of variation (%CV)

23、. For calculation of the GM and %CV, see calculation example for more detail. 6. 第5步中计算得到的X3和3按照以下公式计算得到GM和%CV。GM=eX3%CV=100e3-17. Compare the results of Step 6 to the 2nd Stage of Two Stages acceptance ranges in Table 1. The GM must not fall outside the limits, and the %CV must not be greater than

24、the limit. If both meet the acceptance criteria, the assembly has passed the PVT.第6步计算得到的GM和%CV结果与表格1中“2nd Stage of Two Stages”项下的相应标准比较。GM不能低于范围下限；%CV需要高于限度标准。如果两个结果均符合标准，性能确认通过。In order to comply with the requirements of ASTM E29, all limit values in Table 1 are expressed with two significant figu

25、res.为了满足ASTM E29要求，表格1中标准均用两位有效数字标示。Table 1. Performance Verification Test (PVT) limits (values apply only to Lot R031Y1)性能确认限度标准（批号 R031Y1实验结果）Apparatus方法# of vessels溶出杯数Single-StageTwo-Stage1st Stage of Two Stages2nd Stage of Two StagesGM* %CVGM* %CVGM* %CV1654-841158-808.254-84117812na14na2627-40

26、6.429-364.727-406.376.386.24.86.2126.3na146.2na* Percent of the labeled amount of prednisone dissolved at 30 minutes at 50-rpmCalculation example (expressed as Microsoft Excel worksheet functions): Run 1: x1, x2, ., xn in natural log scale: Ln x1, Ln x2, , Ln xn Run 2: xn+1, xn+2, ., x2n in natural

27、log scale: Ln xn+1, Ln xn+2, , Ln x2n 1st Stage of Two-Stage for n=6, 7, 8 and Single-Stage for n=12, 14: GM1 = exp(average (Ln x1:Ln xn) %CV1 = 100*sqrt(exp(var(Ln x1:Ln xn) -1) Single-Stage or 2nd Stage of Two-Stage for n= 6, 7, 8: GM = exp(average(average (Ln x1:Ln xn), (average (Ln xn+1:Ln x2n)

28、= exp(average (Ln x1:Ln x2n) %CV= 100*sqrt(exp(average(var(Ln x1:Ln xn),(var(Ln xn+1:Ln x2n) -1) exp: exponential (ex ) var: variance sqrt: square root *: multiply 100: conversion factor to percentageNote 1:备注1：There are circumstances when the %CV after the first stage equals or exceeds the value in

29、 the Futility Factor table (without rounding),then it is impossible to meet the %CV criterion after the second stage. The lab can stop after the first stage (run). However, after any adjustments to equipment, test procedure, and so on, the PVT must be restarted with a new first run.双阶实验中：第一阶段实验计算结果中%CV等于或者高出标准上限时，实验终止判定为不合格，不再进行第二阶段实验。再对仪器、检验方法等检查调整后，实验必须重新开始。Futility Factor(%CV at or above value given, second stage testing will not produce passing result)（%CV等于或者大于标准，双阶实验结果不合格）Apparatus方法No. of Vessels溶出杯数678116161628.98.98.8专心-专注-专业