USP潑尼松校正片說明書(中英文對照)

1、Certificate（證書）PREDNISONE TABLETS（潑尼松片）USP Catalog No.: 1559505USP Lot No.: R031Y1(10 mg nominal prednisone content per tablet) （每片含潑尼松10mg）FOR DISSOLUTION PERFORMANCE VERIFICATION TEST (PVT) 用于溶出性能確認(rèn)實(shí)驗(yàn)Period of validity: This certificate of USP Prednisone Tablets Lot R031Y1 is valid through June 30

2、th, 2017.有效期：USP潑尼松片批號R031Y1的證書有效期到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 <711> and DRUG RELEASE <724>, APPARATUS SUITABILITY. Store in

3、a dry place. Store the tablets at controlled room temperature not exceeding 25°.USP潑尼松標(biāo)準(zhǔn)片用于采取USP中方法1和方法2對1升溶出杯，進(jìn)行USP通用測試部分溶出（711）和釋放（724）項(xiàng)目的性能能確認(rèn)實(shí)驗(yàn)，藥品貯藏在干燥，溫度低于25環(huán)境中。Dissolution Medium: We recommend preparing the medium as follows:Heat a suitable amount of water, while stirring gently, to about

4、 41-45°. Filter under vacuum 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 Dissolut

5、ion medium should not fall below 37° prior to the initiation of the test.溶出介質(zhì)：推薦介質(zhì)準(zhǔn)備（操作）如下：（脫氣純化水）加熱適量水同時(shí)輕輕攪拌到約4145。真空下用0.45m濾膜過濾至配有攪拌容器中（即過濾后需要攪拌），密封容器口并繼續(xù)在真空條件下攪拌5分鐘。檢測真空度小于100 mbar。在實(shí)驗(yàn)開始前溶出介質(zhì)溫度不高于37。Procedure：See DISSOLUTION <711> in the current USP: Determine the quantity of prednison

6、e, C21H26O5, dissolvedat 30 minutes, in each vessel, 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 a

7、t 37°. Operate each apparatus at 50- rpm speed. 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

8、Reference Standard.步驟：查看USP現(xiàn)行版的溶出711：確定潑尼松數(shù)量，每個(gè)溶出杯中溶解30分鐘，結(jié)果用百分比表示。499g溶出介質(zhì)（相當(dāng)于500ml溶出介質(zhì)），為了達(dá)到溶出介質(zhì)平衡，實(shí)驗(yàn)開始前不能攪拌溶出介質(zhì)并且溫度控制37。開啟轉(zhuǎn)速50轉(zhuǎn)。30分鐘時(shí)取樣馬上過濾。在242nm波長下測定溶出度（百分比表示）與已知濃度的USP潑尼松參考標(biāo)準(zhǔn)比較。實(shí)驗(yàn)條件：500ml溶出介質(zhì)、37、50轉(zhuǎn)/分鐘、30分鐘取樣檢測： 242nm的波長下測定供試品溶液和對照品溶液的溶出度Note: An amount of alcohol not to exceed 5% of the total

9、 volume of the standard solution may be used to bring 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 pe

10、rformance verification is only required for that apparatus.At the time of use ,peel back the paper-backed lidding to remove the tablets from the blister card注意：1、 乙醇的用量應(yīng)不超過總體積的 1。（對照品先用少量乙醇溶解以加快溶解速度）；2、 自動(dòng)取樣系統(tǒng)可以減少偏差；3、如果只儀器只用一種方法（轉(zhuǎn)籃或槳板），僅僅需要對使用的方法進(jìn)行確認(rèn)；est Interpretation: Laboratory can choose either

11、 of the test schemes listed below.實(shí)驗(yàn)說明：從以下實(shí)驗(yàn)方案中選擇一種Single-Stage Test單階實(shí)驗(yàn)：The following are step-by-step instructions for the Single-Stage test.單階實(shí)驗(yàn)操作步驟：1. For each position in the assembly, test one USP Prednisone Tablets RS, and record the percent dissolved at the sampling time point specified. Tra

12、nsform the percent dissolved results to the natural log scale, determine the mean and variance. For assemblies with 12 or 14 positions (12 or 14 dissolution vessels), no further testing is required.1.每個(gè)溶出杯中放入一粒USP潑尼松片，按照選取方法在規(guī)定時(shí)間點(diǎn)取樣并檢測溶出度。先將各個(gè)溶出度數(shù)據(jù)計(jì)算得到自然對數(shù)，再以自然對數(shù)為數(shù)據(jù)，計(jì)算其平均數(shù)（X1）和方差（1）,12個(gè)和14個(gè)溶出杯的儀器可以不

13、再進(jìn)行后續(xù)檢測。2. For assemblies with fewer than 12 positions, 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個(gè)溶出杯的儀器，重復(fù)第1步操作，即再次向每個(gè)溶出杯中放入一粒USP潑尼松片，按照選取方法在規(guī)定時(shí)間點(diǎn)取樣并檢測溶出度。將檢測得到的各個(gè)溶出杯結(jié)果計(jì)算平

14、均數(shù)（X2）和方差（2）3. Calculate the average of the two means 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將第1、2步中得到的兩個(gè)平均值（X1、X2）和方差（1、2）分別計(jì)算各自的平均值。即X3=X1+X22，3=1+22，（12個(gè)或者14個(gè)溶出杯無需計(jì)算，直接取用第1步計(jì)算結(jié)果，即X3=X1，3=1）4. Convert the

15、 results of Step 3 to a geometric mean (GM) and percent coefficient of variation (%CV). See calculation example below for more detail.4.第3步中計(jì)算得到的X3和3按照以下公式計(jì)算得到GM和%CV。GM=eX3%CV=100×e3-15. Compare the results of Step 4 to the Single-Stage acceptance ranges in Table 1. The GM must not fall outside

16、 the limits,and the %CV must not be greater than the limit. If both meet the criteria, the assembly has passed the PVT.5.第4步計(jì)算得到的GM和%CV結(jié)果與表格1中“Single-Stage”項(xiàng)下的相應(yīng)標(biāo)準(zhǔn)比較。GM不能低于范圍下限；%CV需要高于限度標(biāo)準(zhǔn)。如果兩個(gè)結(jié)果均符合標(biāo)準(zhǔn)，性能確認(rèn)通過。Microsoft Excel中對應(yīng)的各個(gè)計(jì)算公式：自然對數(shù)：LNX：AVERAGE：VAR.SeX: EXPX: SQRTOptional Two-Stage Test：雙階實(shí)驗(yàn)A

17、laboratory may choose to implement the PVT as a Two-Stage test 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

18、two-stage test. 出杯數(shù)量小于12個(gè)的情況下，實(shí)驗(yàn)室可以選擇雙階實(shí)驗(yàn)作為性能確認(rèn)。雙階實(shí)驗(yàn)是一個(gè)有效統(tǒng)計(jì)方法允許第一階段（the first stage）實(shí)驗(yàn)結(jié)果不合格情況下進(jìn)行后續(xù)第二階段實(shí)驗(yàn)（the second stage）。操作步驟如下。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 pe

19、rcent dissolved results to the natural log scale, determine the mean and variance.1.每個(gè)溶出杯中放入一粒USP潑尼松片，按照選取方法在規(guī)定時(shí)間點(diǎn)取樣并檢測溶出度。先將各個(gè)溶出度數(shù)據(jù)計(jì)算得到自然對數(shù)，再以自然對數(shù)為數(shù)據(jù)，計(jì)算其平均數(shù)（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 mu

20、st not fall outside the limits, and the %CV must not be greater than the limit. For calculation of the GM and %CV, see calculation example for more detail. 2. 第1步中計(jì)算得到的X3和3按照以下公式計(jì)算得到GM和%CV。并與表格1中“1st Stage of Two Stages”項(xiàng)下的相應(yīng)標(biāo)準(zhǔn)比較。GM不能低于范圍下限；%CV需要高于限度標(biāo)準(zhǔn)。GM=eX1%CV=100×e1-13. If results of Step 2

21、satisfy both acceptance criteria, the assembly has passed the PVT. Otherwise continue to Step 4. (see note 1).3. 如果第2步兩個(gè)結(jié)果均符合標(biāo)準(zhǔn)，性能確認(rèn)通過，否則需要繼續(xù)第4步操（見備注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

22、and variance for the data obtained at this step.4. 向每個(gè)溶出杯中放入一粒USP潑尼松片，按照選取方法在規(guī)定時(shí)間點(diǎn)取樣并檢測溶出度。將檢測得到的各個(gè)溶出杯結(jié)果計(jì)算平均數(shù)（X2）和方差（2）5. Average the two means and two variances obtained in Steps 1and 4. 將第1步和第4步雙階實(shí)驗(yàn)得到的平均值和方差計(jì)算得平均數(shù)兩個(gè)平均值（X1、X2）和方差（1、2）分別計(jì)算各自的平均值。即X3=X1+X22，3=1+22， 6. Convert the results of Step 5 to

23、 a geometric mean (GM) and percent coefficient of variation (%CV). For calculation of the GM and %CV, see calculation example for more detail. 6. 第5步中計(jì)算得到的X3和3按照以下公式計(jì)算得到GM和%CV。GM=eX3%CV=100×e3-17. Compare the results of Step 6 to the 2nd Stage of Two Stages acceptance ranges in Table 1. The GM

24、must not fall outside the limits, and the %CV must not be greater than the limit. If both meet the acceptance criteria, the assembly has passed the PVT.第6步計(jì)算得到的GM和%CV結(jié)果與表格1中“2nd Stage of Two Stages”項(xiàng)下的相應(yīng)標(biāo)準(zhǔn)比較。GM不能低于范圍下限；%CV需要高于限度標(biāo)準(zhǔn)。如果兩個(gè)結(jié)果均符合標(biāo)準(zhǔn)，性能確認(rèn)通過。In order to comply with the requirements of ASTM E

25、29, all limit values in Table 1 are expressed with two significant figures.為了滿足ASTM E29要求，表格1中標(biāo)準(zhǔn)均用兩位有效數(shù)字標(biāo)示。Table 1. Performance Verification Test (PVT) limits (values apply only to Lot R031Y1)性能確認(rèn)限度標(biāo)準(zhǔn)（批號 R031Y1實(shí)驗(yàn)結(jié)果）Apparatus方法# of vessels溶出杯數(shù)Single-StageTwo-Stage1st Stage of Two Stages2nd Stage of T

26、wo StagesGM* %CVGM* %CVGM* %CV1654-841158-808.254-84117812na14na2627-406.429-364.727-406.376.386.24.86.2126.3na146.2na* Percent of the labeled amount of prednisone dissolved at 30 minutes at 50-rpmCalculation example (expressed as Microsoft ExcelÒ worksheet functions): Run 1: x1, x2, ., xn in n

27、atural log scale: Ln x1, Ln x2, , Ln xn Run 2: xn+1, xn+2, ., x2n in natural 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