[Header] Format=SMU ver=3 appl=GUMWB32 MR=0 FUEB=1 [Title] Title='Assay of Simvastatin in Tablets by HPLC' Description=18 Description[0]='The measurand: mean Simvastatin content of the set of 8 tablets that were taken' Description[1]='as the sample.' Description[2]='' Description[3]='The prototype of the method is based on the monographs of Simvastatin in the' Description[4]='European Pharmacopoeia (Ph.Eur. 5th Ed.) and the United States Pharmacopoeia /' Description[5]='the National Formulary (USP 27 / NF 22).' Description[6]='' Description[7]='Scope of use and validation: Quantitative determination of Simvastatin in drug' Description[8]='products.' Description[9]='' Description[10]='Principle: The drug substance is extracted from the tablets by using solution' Description[11]='of the 0.01M phosphate buffer pH4.0 and acetonitrile in the ratio 20:80 (V/V).' Description[12]='The samples are filtered and the resulting solution is injected into HPLC.' Description[13]='Separation is achieved at room temperature in a Phenomenex Prodigy 3 u ODS' Description[14]='(end-capped) column (30 x 4.60 mm), detection wavelength is 238 nm. A Single' Description[15]='standard solution or a series of calibration solutions (depending on the' Description[16]='calibration procedure) of Simvastatin standard substance is used for' Description[17]='calibration.' [Model] Model=101 Model[0]='{ The main equation' Model[1]=' Calibration graph method (with slope b_1 and intercept b_0) is used for quantitation' Model[2]=' The result is given Recovery-corrected (R)' Model[3]=' The sample solution is prepared by dissolving several tablets to achieve averaging' Model[4]='}' Model[5]='' Model[6]='C_SVT = (A_sample - b_0) * V_100 / ( b_1 * n_tab * R);' Model[7]='' Model[8]='' Model[9]='' Model[10]='{ Chromatographic measurements' Model[11]='Peak areas are used as the basis for quantification.' Model[12]='We assume that the uncertainty of the chromatographic peak area of the sample solution has 4 components' Model[13]=' - Repeatability (contained in A_sample\us\rep)' Model[14]=' - Uncertainty due to detector drift (A_sample\us\drift)' Model[15]=' - Uncertainty due to imperfection of peak integration (A_sample\us\integr)' Model[16]=' - Uncertainty due to the slight nonlinearity of the calibration graph (A_sample\us\nonlin)' Model[17]='The A_sample\us\rep carries the value and the repeatability uncertainty. The other components carry the respective uncertainty component only, their value is 0.' Model[18]='}' Model[19]='' Model[20]='{ Sample peak area }' Model[21]='' Model[22]='A_sample = A_sample\us\rep + A_sample\us\drift + A_sample\us\integr + A_sample\us\nonlin;' Model[23]='' Model[24]='' Model[25]='{ Recovery' Model[26]=' The value of Recovery (R_0) has been determined from spiking studies.' Model[27]=' The R_0 also contains the sample-to-sample variability uncertainty component' Model[28]=' The A_R\us\eff is the effective peak area during recovery determination and it takes into account the uncertainty in determining the recovery value.' Model[29]=' The division by the const() function reforms A_R\us\eff into a coefficient with vaule 1 and uncertainty equal to the relative uncertainty of A_R\us\eff.' Model[30]='}' Model[31]='' Model[32]='R = R_0 * A_R\us\eff / const(A_R\us\eff);' Model[33]='A_R\us\eff = A_R\us\eff\us\integr + A_R\us\eff\us\nonlin;' Model[34]='' Model[35]='' Model[36]='{ Peak areas of the calibration standard solutions' Model[37]=' Their areas have the same components as the sample peak area, except that the nonlinearity uncertainty contribution is not included.' Model[38]='}' Model[39]='' Model[40]='A_1 = A_1rep + A_1drift + A_1integr;' Model[41]='A_2 = A_2rep + A_2drift + A_2integr;' Model[42]='A_3 = A_3rep + A_3drift + A_3integr;' Model[43]='A_4 = A_4rep + A_4drift + A_4integr;' Model[44]='A_5 = A_5rep + A_5drift + A_5integr;' Model[45]='' Model[46]='' Model[47]='' Model[48]='{ Linear regression equations (Calibration graph is used for quantitation) }' Model[49]='' Model[50]='\Sigma\AC = C_1*A_1 + C_2*A_2 + C_3*A_3 +C_4*A_4 + C_5*A_5;' Model[51]='AvgC=(C_1+C_2+C_3+C_4+C_5)/n;' Model[52]='AvgA=(A_1+A_2+A_3+A_4+A_5)/n;' Model[53]='\Sigma\CC=C_1*C_1+C_2*C_2+C_3*C_3+C_4*C_4+C_5*C_5;' Model[54]='b_1=(\Sigma\AC-n*AvgC*AvgA)/(\Sigma\CC-n*AvgC*AvgC);' Model[55]='b_0=AvgA-b_1*AvgC;' Model[56]='' Model[57]='' Model[58]='{ Preparation of standard solutions }' Model[59]='' Model[60]='C_1 = m_1 * P_std / (V_1\us\50 * 100);' Model[61]='C_2 = m_2 * P_std / (V_2\us\50 * 100);' Model[62]='C_3 = m_3 * P_std / (V_3\us\50 * 100);' Model[63]='C_4 = m_4 * P_std / (V_4\us\50 * 100);' Model[64]='C_5 = m_5 * P_std / (V_5\us\50 * 100);' Model[65]='' Model[66]='' Model[67]='{ Uncertainity of weighing' Model[68]='}' Model[69]='' Model[70]='m_1 = m_1\us\rep + m_1\us\buoyancy + m_1\us\drift + m_1\us\round + m_1\us\electrost;' Model[71]='m_2 = m_2\us\rep + m_2\us\buoyancy + m_2\us\drift + m_2\us\round + m_2\us\electrost;' Model[72]='m_3 = m_3\us\rep + m_3\us\buoyancy + m_3\us\drift + m_3\us\round + m_3\us\electrost;' Model[73]='m_4 = m_4\us\rep + m_4\us\buoyancy + m_4\us\drift + m_4\us\round + m_4\us\electrost;' Model[74]='m_5 = m_5\us\rep + m_5\us\buoyancy + m_5\us\drift + m_5\us\round + m_5\us\electrost;' Model[75]='' Model[76]='m_1\us\buoyancy = m_1\us\rep * f_buoyancy;' Model[77]='m_2\us\buoyancy = m_2\us\rep * f_buoyancy;' Model[78]='m_3\us\buoyancy = m_3\us\rep * f_buoyancy;' Model[79]='m_4\us\buoyancy = m_4\us\rep * f_buoyancy;' Model[80]='m_5\us\buoyancy = m_5\us\rep * f_buoyancy;' Model[81]='' Model[82]='' Model[83]='{ Volumes of 50 ml volumetric flask }' Model[84]='' Model[85]='V_1\us\50 = V_1\us\50\us\cal + V_1\us\50\us\fill + V_1\us\50\us\temp;' Model[86]='V_2\us\50 = V_2\us\50\us\cal + V_2\us\50\us\fill + V_2\us\50\us\temp;' Model[87]='V_3\us\50 = V_3\us\50\us\cal + V_3\us\50\us\fill + V_3\us\50\us\temp;' Model[88]='V_4\us\50 = V_4\us\50\us\cal + V_4\us\50\us\fill + V_4\us\50\us\temp;' Model[89]='V_5\us\50 = V_5\us\50\us\cal + V_5\us\50\us\fill + V_5\us\50\us\temp;' Model[90]='V_1\us\50\us\temp = V_1\us\50\us\cal * \Delta\t * \gamma\_w;' Model[91]='V_2\us\50\us\temp = V_2\us\50\us\cal * \Delta\t * \gamma\_w;' Model[92]='V_3\us\50\us\temp = V_3\us\50\us\cal * \Delta\t * \gamma\_w;' Model[93]='V_4\us\50\us\temp = V_4\us\50\us\cal * \Delta\t * \gamma\_w;' Model[94]='V_5\us\50\us\temp = V_5\us\50\us\cal * \Delta\t * \gamma\_w;' Model[95]='' Model[96]='' Model[97]='{ Volume of the sample solution }' Model[98]='' Model[99]='V_100 = V_100\us\cal + V_100\us\fill + V_100\us\temp;' Model[100]='V_100\us\temp = V_100\us\cal * \Delta\t * \gamma\_w;' CE=1 CTC=1 [Components] CompOrder=1 Comp=102 Comp[0]=A_1_ Comp[1]=A_1drift_ Comp[2]=A_1integr_ Comp[3]=A_1rep_ Comp[4]=A_2_ Comp[5]=A_2drift_ Comp[6]=A_2integr_ Comp[7]=A_2rep_ Comp[8]=A_3_ Comp[9]=A_3drift_ Comp[10]=A_3integr_ Comp[11]=A_3rep_ Comp[12]=A_4_ Comp[13]=A_4drift_ Comp[14]=A_4integr_ Comp[15]=A_4rep_ Comp[16]=A_5_ Comp[17]=A_5drift_ Comp[18]=A_5integr_ Comp[19]=A_5rep_ Comp[20]=A_R\us\eff_ Comp[21]=A_R\us\eff\us\integr_ Comp[22]=A_R\us\eff\us\nonlin_ Comp[23]=A_sample_ Comp[24]=A_sample\us\drift_ Comp[25]=A_sample\us\integr_ Comp[26]=A_sample\us\nonlin_ Comp[27]=A_sample\us\rep_ Comp[28]=AvgA Comp[29]=AvgC Comp[30]=b_0_ Comp[31]=b_1_ Comp[32]=C_1_ Comp[33]=C_2_ Comp[34]=C_3_ Comp[35]=C_4_ Comp[36]=C_5_ Comp[37]=C_SVT_ Comp[38]=f_buoyancy_ Comp[39]=m_1_ Comp[40]=m_1\us\buoyancy_ Comp[41]=m_1\us\drift_ Comp[42]=m_1\us\electrost_ Comp[43]=m_1\us\rep_ Comp[44]=m_1\us\round_ Comp[45]=m_2_ Comp[46]=m_2\us\buoyancy_ Comp[47]=m_2\us\drift_ Comp[48]=m_2\us\electrost_ Comp[49]=m_2\us\rep_ Comp[50]=m_2\us\round_ Comp[51]=m_3_ Comp[52]=m_3\us\buoyancy_ Comp[53]=m_3\us\drift_ Comp[54]=m_3\us\electrost_ Comp[55]=m_3\us\rep_ Comp[56]=m_3\us\round_ Comp[57]=m_4_ Comp[58]=m_4\us\buoyancy_ Comp[59]=m_4\us\drift_ Comp[60]=m_4\us\electrost_ Comp[61]=m_4\us\rep_ Comp[62]=m_4\us\round_ Comp[63]=m_5_ Comp[64]=m_5\us\buoyancy_ Comp[65]=m_5\us\drift_ Comp[66]=m_5\us\electrost_ Comp[67]=m_5\us\rep_ Comp[68]=m_5\us\round_ Comp[69]=n Comp[70]=n_tab_ Comp[71]=P_std_ Comp[72]=R Comp[73]=R_0_ Comp[74]=V_100_ Comp[75]=V_100\us\cal_ Comp[76]=V_100\us\fill_ Comp[77]=V_100\us\temp_ Comp[78]=V_1\us\50_ Comp[79]=V_1\us\50\us\cal_ Comp[80]=V_1\us\50\us\fill_ Comp[81]=V_1\us\50\us\temp_ Comp[82]=V_2\us\50_ Comp[83]=V_2\us\50\us\cal_ Comp[84]=V_2\us\50\us\fill_ Comp[85]=V_2\us\50\us\temp_ Comp[86]=V_3\us\50_ Comp[87]=V_3\us\50\us\cal_ Comp[88]=V_3\us\50\us\fill_ Comp[89]=V_3\us\50\us\temp_ Comp[90]=V_4\us\50_ Comp[91]=V_4\us\50\us\cal_ Comp[92]=V_4\us\50\us\fill_ Comp[93]=V_4\us\50\us\temp_ Comp[94]=V_5\us\50_ Comp[95]=V_5\us\50\us\cal_ Comp[96]=V_5\us\50\us\fill_ Comp[97]=V_5\us\50\us\temp_ Comp[98]=\Delta\t Comp[99]=\gamma\_w_ Comp[100]=\Sigma\AC Comp[101]=\Sigma\CC [COMP 0] Type=Temp Definition='Peak area of the 1. calibration standard solution' Unit='AU' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=4407267 Ustd=21071.3075057055 Neff=114 HB=1 HC=0 HR=1 IO=0 [COMP 1] Type=TypBRectang Definition='Drift uncertainty component of the peak area of the 1. calibration standard solution' Unit='AU' Description=4 Description[0]='The drift per hour is maximum 12 000 peak area units. Assuming that the' Description[1]='solution will be kept no longer than 2 hours between preparation and' Description[2]='measurement we arrive at this uncertainty estimate. This uncertainty estimate' Description[3]='is essentially independent of the peak area.' Vnom=0 Hlim=24000 [COMP 2] Type=TypBRectang Definition='Integration uncertainty component of the peak area of the 1. calibration standard solution' Unit='AU' Description=5 Description[0]='This uncertainty contribution has been obtained by integrating the peak in two' Description[1]='ways - one somewhat underestimating (Area(min)) and the other somewhat' Description[2]='overestimating (Area(max)) the peak area. The uncertainty contribution has been' Description[3]='taken equal to [Area(max)-Area(min)]/2. See text for more detail. According to' Description[4]='our data this uncertainty contribution is proportional to the peak area.' Vnom=0 Hlim=18000 [COMP 3] Type=TypASum Definition='Value and the repeatability uncertainty component of the peak area of the 1. calibration standard solution' Unit='AU' Description=5 Description[0]='The repeatability uncertainty has been estimated using the pooled standard' Description[1]='deviation of triplicate injections (altogether 3 x 6 injections) of a standard' Description[2]='solution subjected to different stability tests. See the text for more detail.' Description[3]='According to our data this uncertainty contribution is essentially independent' Description[4]='of the sample peak area.' Vnom=4407267 Ustd=12000 Neff=12 [COMP 4] Type=Temp Definition='Peak area of the 2. calibration standard solution' Unit='AU' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=6436226 Ustd=28936.7125522809 Neff=405 HB=1 HC=0 HR=1 IO=0 [COMP 5] Type=TypBRectang Definition='Drift uncertainty component of the peak area of the 2. calibration standard solution' Unit='AU' Description=4 Description[0]='The drift per hour is maximum 12 000 peak area units. Assuming that the' Description[1]='solution will be kept no longer than 3 hours between preparation and' Description[2]='measurement we arrive at this uncertainty estimate. This uncertainty estimate' Description[3]='is essentially independent of the peak area.' Vnom=0 Hlim=36000 [COMP 6] Type=TypBRectang Definition='Integration uncertainty component of the peak area of the 2. calibration standard solution' Unit='AU' Description=5 Description[0]='This uncertainty contribution has been obtained by integrating the peak in two' Description[1]='ways - one somewhat underestimating (Area(min)) and the other somewhat' Description[2]='overestimating (Area(max)) the peak area. The uncertainty contribution has been' Description[3]='taken equal to [Area(max)-Area(min)]/2. See text for more detail. According to' Description[4]='our data this uncertainty contribution is proportional to the peak area.' Vnom=0 Hlim=28000 [COMP 7] Type=TypASum Definition='Value and the repeatability uncertainty component of the peak area of the 2. calibration standard solution' Unit='AU' Description=5 Description[0]='The repeatability uncertainty has been estimated using the pooled standard' Description[1]='deviation of triplicate injections (altogether 3 x 6 injections) of a standard' Description[2]='solution subjected to different stability tests. See the text for more detail.' Description[3]='According to our data this uncertainty contribution is essentially independent' Description[4]='of the sample peak area.' Vnom=6436226 Ustd=12000 Neff=12 [COMP 8] Type=Temp Definition='Peak area of the 3. calibration standard solution' Unit='AU' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=8987202 Ustd=37497.7777119303 Neff=1144 HB=1 HC=0 HR=1 IO=0 [COMP 9] Type=TypBRectang Definition='Drift uncertainty component of the peak area of the 3. calibration standard solution' Unit='AU' Description=4 Description[0]='The drift per hour is maximum 12 000 peak area units. Assuming that the' Description[1]='solution will be kept no longer than 4 hours between preparation and' Description[2]='measurement we arrive at this uncertainty estimate. This uncertainty estimate' Description[3]='is essentially independent of the peak area.' Vnom=0 Hlim=48000 [COMP 10] Type=TypBRectang Definition='Integration uncertainty component of the peak area of the 3. calibration standard solution' Unit='AU' Description=5 Description[0]='This uncertainty contribution has been obtained by integrating the peak in two' Description[1]='ways - one somewhat underestimating (Area(min)) and the other somewhat' Description[2]='overestimating (Area(max)) the peak area. The uncertainty contribution has been' Description[3]='taken equal to [Area(max)-Area(min)]/2. See text for more detail. According to' Description[4]='our data this uncertainty contribution is proportional to the peak area.' Vnom=0 Hlim=38500 [COMP 11] Type=TypASum Definition='Value and the repeatability uncertainty component of the peak area of the 3. calibration standard solution' Unit='AU' Description=5 Description[0]='The repeatability uncertainty has been estimated using the pooled standard' Description[1]='deviation of triplicate injections (altogether 3 x 6 injections) of a standard' Description[2]='solution subjected to different stability tests. See the text for more detail.' Description[3]='According to our data this uncertainty contribution is essentially independent' Description[4]='of the sample peak area.' Vnom=8987202 Ustd=12000 Neff=12 [COMP 12] Type=Temp Definition='Peak area of the 4. calibration standard solution' Unit='AU' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=10642449.5 Ustd=45610.6712659804 Neff=2504 HB=1 HC=0 HR=1 IO=0 [COMP 13] Type=TypBRectang Definition='Drift uncertainty component of the peak area of the 4. calibration standard solution' Unit='AU' Description=4 Description[0]='The drift per hour is maximum 12 000 peak area units. Assuming that the' Description[1]='solution will be kept no longer than 5 hours between preparation and' Description[2]='measurement we arrive at this uncertainty estimate. This uncertainty estimate' Description[3]='is essentially independent of the peak area.' Vnom=0 Hlim=60000 [COMP 14] Type=TypBRectang Definition='Integration uncertainty component of the peak area of the 4. calibration standard solution' Unit='AU' Description=5 Description[0]='This uncertainty contribution has been obtained by integrating the peak in two' Description[1]='ways - one somewhat underestimating (Area(min)) and the other somewhat' Description[2]='overestimating (Area(max)) the peak area. The uncertainty contribution has been' Description[3]='taken equal to [Area(max)-Area(min)]/2. See text for more detail. According to' Description[4]='our data this uncertainty contribution is proportional to the peak area.' Vnom=0 Hlim=47000 [COMP 15] Type=TypASum Definition='Value and the repeatability uncertainty component of the peak area of the 4. calibration standard solution' Unit='AU' Description=5 Description[0]='The repeatability uncertainty has been estimated using the pooled standard' Description[1]='deviation of triplicate injections (altogether 3 x 6 injections) of a standard' Description[2]='solution subjected to different stability tests. See the text for more detail.' Description[3]='According to our data this uncertainty contribution is essentially independent' Description[4]='of the sample peak area.' Vnom=10642449.5 Ustd=12000 Neff=12 [COMP 16] Type=Temp Definition='Peak area of the 5. calibration standard solution' Unit='AU' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=13070522 Ustd=54535.1568562275 Neff=5118 HB=1 HC=0 HR=1 IO=0 [COMP 17] Type=TypBRectang Definition='Drift uncertainty component of the peak area of the 5. calibration standard solution' Unit='AU' Description=4 Description[0]='The drift per hour is maximum 12 000 peak area units. Assuming that the' Description[1]='solution will be kept no longer than 6 hours between preparation and' Description[2]='measurement we arrive at this uncertainty estimate. This uncertainty estimate' Description[3]='is essentially independent of the peak area.' Vnom=0 Hlim=72000 [COMP 18] Type=TypBRectang Definition='Integration uncertainty component of the peak area of the 5. calibration standard solution' Unit='AU' Description=5 Description[0]='This uncertainty contribution has been obtained by integrating the peak in two' Description[1]='ways - one somewhat underestimating (Area(min)) and the other somewhat' Description[2]='overestimating (Area(max)) the peak area. The uncertainty contribution has been' Description[3]='taken equal to [Area(max)-Area(min)]/2. See text for more detail. According to' Description[4]='our data this uncertainty contribution is proportional to the peak area.' Vnom=0 Hlim=57500 [COMP 19] Type=TypASum Definition='Value and the repeatability uncertainty component of the peak area of the 5. calibration standard solution' Unit='AU' Description=5 Description[0]='The repeatability uncertainty has been estimated using the pooled standard' Description[1]='deviation of triplicate injections (altogether 3 x 6 injections) of a standard' Description[2]='solution subjected to different stability tests. See the text for more detail.' Description[3]='According to our data this uncertainty contribution is essentially independent' Description[4]='of the sample peak area.' Vnom=13070522 Ustd=12000 Neff=12 [COMP 20] Type=Temp Definition='The effective peak area during the Recovery determination (difference of the peak areas of spiked and unspiked solutions)' Unit='AU' Description=7 Description[0]='The systemati influences are practically limited to the systematic effects in' Description[1]='peak areas (repeatability can thus be excluded). Also, it is necessary to keep' Description[2]='in mind that calculation of Recovery by spiking experiments leads to' Description[3]='differences of areas of peaks that have been obtained within short time' Description[4]='intervals (the drift component can thus be excluded). Therefore the components' Description[5]='to be included are the integration uncertainty and the uncertainty due to' Description[6]='nonlinearity.' Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=3000000 Ustd=24212.6688601925 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 21] Type=TypBRectang Definition='The value and integration uncertainty of the effective peak area during the recovery determination' Unit='AU' Description=0 Vnom=3000000 Hlim=12600 [COMP 22] Type=TypBRectang Definition='The uncertainty of the effective peak area due to nonlinearity of the calibration graph during the recovery determination' Unit='AU' Description=0 Vnom=0 Hlim=40000 [COMP 23] Type=Temp Definition='Peak area of the sample solution' Unit='AU' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=8349089 Ustd=50026.6595593456 Neff=1345 HB=0 HC=0 HR=0 IO=0 [COMP 24] Type=TypBRectang Definition='Drift uncertainty component of the sample peak area' Unit='AU' Description=4 Description[0]='The drift per hour is maximum 12 000 peak area units. Assuming that the sample' Description[1]='solution will be kept no longer than 5 hours between preparation and' Description[2]='measurement we arrive at this uncertainty estimate. This uncertainty estimate' Description[3]='is essentially independent of the peak area.' Vnom=0 Hlim=60000 [COMP 25] Type=TypBRectang Definition='Integration uncertainty component of the sample peak area' Unit='AU' Description=5 Description[0]='This uncertainty contribution has been obtained by integrating the peak in two' Description[1]='ways - one somewhat underestimating (Area(min)) and the other somewhat' Description[2]='overestimating (Area(max)) the peak area. The uncertainty contribution has been' Description[3]='taken equal to [Area(max)-Area(min)]/2. See text for more detail. According to' Description[4]='our data this uncertainty contribution is proportional to the peak area.' Vnom=0 Hlim=35000 [COMP 26] Type=TypBRectang Definition='Uncertainty component of the sample peak area that takes into account the slight non-linearity of the calibration graph' Unit='AU' Description=7 Description[0]='This uncertainty contribution has been estimated from the behavior of the' Description[1]='residuals of the calibration line. The uncertainty corresponds to the maximum' Description[2]='possible devaition (in terms of peak area) of the calibration line from the' Description[3]='actual concentration vs peak area relationship. This uncertainty contribution' Description[4]='is assigned only to the peak area of the sample and not to the peak areas of' Description[5]='the standard solutions. According to this approach this uncertainty' Description[6]='countribution is assumed to be independent of the peak area of the sample.' Vnom=0 Hlim=40000 [COMP 27] Type=TypASum Definition='The value of the sample solution peak area together with its repeatability uncertainty' Unit='AU' Description=5 Description[0]='The repeatability uncertainty has been estimated using the pooled standard' Description[1]='deviation of triplicate injections (altogether 3 x 14 injections) of a sample' Description[2]='solution subjected to different stability tests. See the text for more detail.' Description[3]='According to our data this uncertainty contribution is essentially independent' Description[4]='of the sample peak area.' Vnom=8349089 Ustd=19000 Neff=28 [COMP 28] Type=Temp Definition='Interim quantity for regression statistics calculation' Unit='AU' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=8708733.3 Ustd=28032.7189786031 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 29] Type=Temp Definition='Interim quantity for regression statistics calculation' Unit='mg/ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=0.80900972152 Ustd=0.00361080973943389 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 30] Type=Temp Definition='Intercept of the calibration line' Unit='AU' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=145855.3410348 Ustd=38325.133299416 Neff=999 HB=0 HC=0 HR=0 IO=0 [COMP 31] Type=Temp Definition='Slope of the calibration line' Unit='AU*ml/mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=10584394.3913021 Ustd=77774.2352067926 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 32] Type=Temp Definition='Concentration of the 1. calibration standard solution' Unit='mg/ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=0.4063555496 Ustd=0.0019529750173156 Neff=7358 HB=0 HC=0 HR=0 IO=0 [COMP 33] Type=Temp Definition='Concentration of the 2. calibration standard solution' Unit='mg/ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=0.5914244336 Ustd=0.00283505242291524 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 34] Type=Temp Definition='Concentration of the 3. calibration standard solution' Unit='mg/ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=0.8322129816 Ustd=0.00395807686561459 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 35] Type=Temp Definition='Concentration of the 4. calibration standard solution' Unit='mg/ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=0.9916110204 Ustd=0.004706051782186 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 36] Type=Temp Definition='Concentration of the 5. calibration standard solution' Unit='mg/ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=1.2234446224 Ustd=0.00580852379478739 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 37] Type=Result Definition='Content of simvastatin in Simvastatin 10 mg tablets' Unit='mg/tab' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=9.66789416434567 Ustd=0.11376993463709 Neff=1296 HB=1 HC=0 HR=1 IO=0 [COMP 38] Type=TypBRectang Definition='Correction factor for air buoyancy' Unit='unitless' Description=4 Vnom=0.0010 Hlim=0.0002 Description[0]='The buoyancy factor is the part (around one thousandth under our conditions) of' Description[1]='the mass that is added to the balance reading in order to get the physical mass' Description[2]='of the weighed substance. The uncertainty estimate is deliberately very' Description[3]='conservative.' [COMP 39] Type=Temp Definition='Mass of the Simvastatin CRS taken for preparation of the 1. calibration standard solution' Unit='mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=20.44042 Ustd=0.0618566492477567 Neff=1156 HB=0 HC=0 HR=0 IO=0 [COMP 40] Type=Temp Definition='Air buoyancy component of uncertainity of mass m1' Unit='mg' Description=0 Vnom=0.02042 Ustd=0.00235797996033328 Neff=10000 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 HB=0 HC=0 HR=0 IO=0 [COMP 41] Type=TypASum Definition='Drift component of uncertainity of mass m1' Unit='mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=0 Ustd=0.0097 Neff=2 HB=0 HC=0 HR=0 IO=0 [COMP 42] Type=TypBRectang Definition='Electrostatic component of uncertainity of mass m1' Unit='mg' Description=4 Vnom=0 Ustd=0.0097 Neff=2 Description[0]='When weighing the standard substance, intereference from electrostatics' Description[1]='(instability of the reading) was quite serious and is thus taken into account' Description[2]='as an uncertainty component. This uncertainty componen has been estimated as' Description[3]='0.5% of the mass of the substance.' Hlim=0.10 [COMP 43] Type=TypASum Definition='Value of the mass of the Simvastatin CRS taken for preparation of the 1. calibration standard solution together with repeatability component of uncertainity' Unit='mg' Description=0 Description[0]='When weighing the standard substance, intereference from electrostatics' Description[1]='(instability of the reading) was quite serious and is thus taken into account' Description[2]='as an uncertainty component. This uncertainty componen has been estimated as' Description[3]='0.5% of the mass of the substance.' Vnom=20.42 Hlim=0.10 Ustd=0.0196 Neff=18 [COMP 44] Type=TypBRectang Definition='Rounding component of uncertainity of mass m1' Unit='mg' Description=0 Vnom=0 Hlim=0.005 [COMP 45] Type=Temp Definition='Mass of the Simvastatine CRS taken for preparation of the 2. calibration standard solution' Unit='mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=29.74972 Ustd=0.0894378503924746 Neff=5054 HB=0 HC=0 HR=0 IO=0 [COMP 46] Type=Temp Definition='Air buoyancy component of uncertainity of mass m2' Unit='mg' Description=0 Vnom=0.02972 Ustd=0.00343182597072365 Neff=10000 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 HB=0 HC=0 HR=0 IO=0 [COMP 47] Type=TypASum Definition='Drift component of uncertainity of mass m2' Unit='mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=0 Ustd=0.0097 Neff=2 HB=0 HC=0 HR=0 IO=0 [COMP 48] Type=TypBRectang Definition='Electrostatic component of uncertainity of mass m2' Unit='mg' Description=4 Vnom=0 Ustd=0.0097 Neff=2 Description[0]='When weighing the standard substance, intereference from electrostatics' Description[1]='(instability of the reading) was quite serious and is thus taken into account' Description[2]='as an uncertainty component. This uncertainty componen has been estimated as' Description[3]='0.5% of the mass of the substance.' Hlim=0.15 [COMP 49] Type=TypASum Definition='Value of the mass of the Simvastatine CRS taken for preparation of the 2. calibration standard solution together with repeatability component of uncertainity' Unit='mg' Description=0 Description[0]='When weighing the standard substance, intereference from electrostatics' Description[1]='(instability of the reading) was quite serious and is thus taken into account' Description[2]='as an uncertainty component. This uncertainty componen has been estimated as' Description[3]='0.5% of the mass of the substance.' Vnom=29.72 Hlim=0.15 Ustd=0.0196 Neff=18 [COMP 50] Type=TypBRectang Definition='Rounding component of uncertainity of mass m2' Unit='mg' Description=0 Vnom=0 Hlim=0.005 [COMP 51] Type=Temp Definition='Mass of the Simvastatine CRS taken for preparation of the 3. calibration standard solution' Unit='mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=41.86182 Ustd=0.123331548557104 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 52] Type=Temp Definition='Air buoyancy component of uncertainity of mass m3' Unit='mg' Description=0 Vnom=0.04182 Ustd=0.00482899742803825 Neff=10000 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 HB=0 HC=0 HR=0 IO=0 [COMP 53] Type=TypASum Definition='Drift component of uncertainity of mass m3' Unit='mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=0 Ustd=0.0097 Neff=2 HB=0 HC=0 HR=0 IO=0 [COMP 54] Type=TypBRectang Definition='Electrostatic component of uncertainity of mass m3' Unit='mg' Description=4 Vnom=0 Ustd=0.0097 Neff=2 Description[0]='When weighing the standard substance, intereference from electrostatics' Description[1]='(instability of the reading) was quite serious and is thus taken into account' Description[2]='as an uncertainty component. This uncertainty componen has been estimated as' Description[3]='0.5% of the mass of the substance.' Hlim=0.21 [COMP 55] Type=TypASum Definition='Value of the mass of the Simvastatine CRS taken for preparation of the 3. calibration standard solution together with repeatability component of uncertainity' Unit='mg' Description=0 Description[0]='When weighing the standard substance, intereference from electrostatics' Description[1]='(instability of the reading) was quite serious and is thus taken into account' Description[2]='as an uncertainty component. This uncertainty componen has been estimated as' Description[3]='0.5% of the mass of the substance.' Vnom=41.82 Hlim=0.21 Ustd=0.0196 Neff=18 [COMP 56] Type=TypBRectang Definition='Rounding component of uncertainity of mass m3' Unit='mg' Description=0 Vnom=0 Hlim=0.005 [COMP 57] Type=Temp Definition='Mass of the Simvastatine CRS taken for preparation of the 4. calibration standard solution' Unit='mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=49.87983 Ustd=0.146129368789531 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 58] Type=Temp Definition='Air buoyancy component of uncertainity of mass m4' Unit='mg' Description=0 Vnom=0.04983 Ustd=0.00575390616538018 Neff=10000 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 HB=0 HC=0 HR=0 IO=0 [COMP 59] Type=TypASum Definition='Drift component of uncertainity of mass m4' Unit='mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=0 Ustd=0.0097 Neff=2 HB=0 HC=0 HR=0 IO=0 [COMP 60] Type=TypBRectang Definition='Electrostatic component of uncertainity of mass m4' Unit='mg' Description=4 Vnom=0 Ustd=0.0097 Neff=2 Description[0]='When weighing the standard substance, intereference from electrostatics' Description[1]='(instability of the reading) was quite serious and is thus taken into account' Description[2]='as an uncertainty component. This uncertainty componen has been estimated as' Description[3]='0.5% of the mass of the substance.' Hlim=0.25 [COMP 61] Type=TypASum Definition='Value of the mass of the Simvastatine CRS taken for preparation of the 4. calibration standard solution together with repeatability component of uncertainity' Unit='mg' Description=0 Description[0]='When weighing the standard substance, intereference from electrostatics' Description[1]='(instability of the reading) was quite serious and is thus taken into account' Description[2]='as an uncertainty component. This uncertainty componen has been estimated as' Description[3]='0.5% of the mass of the substance.' Vnom=49.83 Hlim=0.25 Ustd=0.0196 Neff=18 [COMP 62] Type=TypBRectang Definition='Rounding component of uncertainity of mass m4' Unit='mg' Description=0 Vnom=0 Hlim=0.005 [COMP 63] Type=Temp Definition='Mass of the Simvastatine CRS taken for preparation of the 5. calibration standard solution' Unit='mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=61.54148 Ustd=0.180474603687499 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 64] Type=Temp Definition='Air buoyancy component of uncertainity of mass m5' Unit='mg' Description=0 Vnom=0.06148 Ustd=0.00709912596685911 Neff=10000 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 HB=0 HC=0 HR=0 IO=0 [COMP 65] Type=TypASum Definition='Drift component of uncertainity of mass m5' Unit='mg' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=0 Ustd=0.0097 Neff=2 HB=0 HC=0 HR=0 IO=0 [COMP 66] Type=TypBRectang Definition='Electrostatic component of uncertainity of mass m5' Unit='mg' Description=4 Vnom=0 Ustd=0.0097 Neff=2 Description[0]='When weighing the standard substance, intereference from electrostatics' Description[1]='(instability of the reading) was quite serious and is thus taken into account' Description[2]='as an uncertainty component. This uncertainty componen has been estimated as' Description[3]='0.5% of the mass of the substance.' Hlim=0.31 [COMP 67] Type=TypASum Definition='Value of the mass of the Simvastatine CRS taken for preparation of the 5. calibration standard solution together with repeatability component of uncertainity' Unit='mg' Description=0 Description[0]='When weighing the standard substance, intereference from electrostatics' Description[1]='(instability of the reading) was quite serious and is thus taken into account' Description[2]='as an uncertainty component. This uncertainty componen has been estimated as' Description[3]='0.5% of the mass of the substance.' Vnom=61.48 Hlim=0.31 Ustd=0.0196 Neff=18 [COMP 68] Type=TypBRectang Definition='Rounding component of uncertainity of mass m5' Unit='mg' Description=0 Vnom=0 Hlim=0.005 [COMP 69] Type=Const Definition='Number of points on the calibration line' Unit='unitless' Description=0 Vnom=5 [COMP 70] Type=Const Definition='Number of the tablets taken for preparation of the sample solution' Unit='tab' Description=0 Vnom=8 [COMP 71] Type=TypBRectang Definition='Purity of the Simvastatin CRS' Unit='%' Description=0 Vnom=99.4 Hlim=0.6 [COMP 72] Type=Temp Definition='Recovery' Unit='unitless' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=1.002068 Ustd=0.00840690066621909 Neff=360 HB=0 HC=0 HR=0 IO=0 [COMP 73] Type=TypASum Definition='The value of R and its uncertainty component that is due to the imperfection of the sample preparation procedure' Unit='unitless' Description=3 Description[0]='Recovery value and sample-to-sample variability uncertainty. The standard' Description[1]='uncertainty is the standard deviation of the single mavlue, not the standard' Description[2]='deviation of the mean' Vnom=1.002068 Ustd=0.002295 Neff=2 [COMP 74] Type=Temp Definition='Volume of the sample solution' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=100 Ustd=0.091571465715764 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 75] Type=TypBRectang Definition='Value of the volume of the sample solution together with calibration component of uncertainity' Unit='ml' Description=0 Vnom=100.00 Hlim=0.1 [COMP 76] Type=TypBRectang Definition='Filling component of uncertainity of volume V_100' Unit='ml' Description=0 Vnom=0 Hlim=0.09 [COMP 77] Type=Temp Definition='Uncertainity component of volume V_100 due to temperature difference from 20°C' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=0 Ustd=0.0484974226119286 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 78] Type=Temp Definition='Volume of the 1. calibration standard solution' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=50 Ustd=0.0669925368977769 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 79] Type=TypBRectang Definition='Value of the volume of the 1. calibration standard solution together with calibration component of uncertainity' Unit='ml' Description=0 Vnom=50.00 Hlim=0.06 [COMP 80] Type=TypBRectang Definition='Filling component of uncertainity of volume V_1\us\50' Unit='ml' Description=0 Vnom=0 Hlim=0.09 [COMP 81] Type=Temp Definition='Uncertainity component of volume V_1\us\50 due to temperature difference from 20°C' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=0 Ustd=0.0242487113059643 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 82] Type=Temp Definition='Volume of the 2. calibration standard solution' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=50 Ustd=0.0669925368977769 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 83] Type=TypBRectang Definition='Value of the volume of the 2. calibration standard solution together with calibration component of uncertainity' Unit='ml' Description=0 Vnom=50.00 Hlim=0.06 [COMP 84] Type=TypBRectang Definition='Filling component of uncertainity of volume V_2\us\50' Unit='ml' Description=0 Vnom=0 Hlim=0.09 [COMP 85] Type=Temp Definition='Uncertainity component of volume V_2\us\50 due to temperature difference from 20°C' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=0 Ustd=0.0242487113059643 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 86] Type=Temp Definition='Volume of the 3. calibration standard solution' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=50 Ustd=0.0669925368977769 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 87] Type=TypBRectang Definition='Value of the volume of the 3. calibration standard solution together with calibration component of uncertainity' Unit='ml' Description=0 Vnom=50.00 Hlim=0.06 [COMP 88] Type=TypBRectang Definition='Filling component of uncertainity of volume V_3\us\50' Unit='ml' Description=0 Vnom=0 Hlim=0.09 [COMP 89] Type=Temp Definition='Uncertainity component of volume V_3\us\50 due to temperature difference from 20°C' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=0 Ustd=0.0242487113059643 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 90] Type=Temp Definition='Volume of the 4. calibration standard solution' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=50 Ustd=0.0669925368977769 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 91] Type=TypBRectang Definition='Value of the volume of the 4. calibration standard solution together with calibration component of uncertainity' Unit='ml' Description=0 Vnom=50.00 Hlim=0.06 [COMP 92] Type=TypBRectang Definition='Filling component of uncertainity of volume V_4\us\50' Unit='ml' Description=0 Vnom=0 Hlim=0.09 [COMP 93] Type=Temp Definition='Uncertainity component of volume V_4\us\50 due to temperature difference from 20°C' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=0 Ustd=0.0242487113059643 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 94] Type=Temp Definition='Volume of the 5. calibration standard solution' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=50 Ustd=0.0669925368977769 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 95] Type=TypBRectang Definition='Value of the volume of the 5. calibration standard solution together with calibration component of uncertainity' Unit='ml' Description=0 Vnom=50.00 Hlim=0.06 [COMP 96] Type=TypBRectang Definition='Filling component of uncertainity of volume V_5\us\50' Unit='ml' Description=0 Vnom=0 Hlim=0.09 [COMP 97] Type=Temp Definition='Uncertainity component of volume V_5\us\50 due to temperature difference from 20°C' Unit='ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=0 Ustd=0.0242487113059643 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 98] Type=TypBRectang Definition='Diference of solution temperature from 20°C' Unit='°C' Description=0 Vnom=0 Hlim=4 [COMP 99] Type=Const Definition='Thermal expansion coefficent of water' Unit='1/°C' Description=0 Vnom=0.00021 [COMP 100] Type=Temp Definition='Interim quantity for regression statistics' Unit='AU*mg/ml' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=39620954.9543634 Ustd=220353.831877012 Neff=10000 HB=0 HC=0 HR=0 IO=0 [COMP 101] Type=Temp Definition='Interim quantity for regression statistics' Unit='mg²/ml²' Description=0 Fcov=2 NomUnit= UncUnit= CovID=0 UncID=0 Vnom=3.68759529995157 Ustd=0.0330742770821377 Neff=10000 HB=0 HC=0 HR=0 IO=0 [Correlations] Coefficient[1,5]=0.8 Coefficient[1,9]=0.8 Coefficient[1,13]=0.8 Coefficient[1,17]=0.8 Coefficient[5,9]=0.8 Coefficient[5,13]=0.8 Coefficient[9,13]=0.8 Coefficient[5,17]=0.8 Coefficient[9,17]=0.8 Coefficient[13,17]=0.8 Coefficient[42,48]=0.8 Coefficient[42,54]=0.8 Coefficient[42,60]=0.8 Coefficient[42,66]=0.8 Coefficient[48,54]=0.8 Coefficient[48,60]=0.8 Coefficient[48,66]=0.8 Coefficient[54,60]=0.8 Coefficient[54,66]=0.8 Coefficient[60,66]=0.8 Coefficient[43,49]=0.8 Coefficient[43,55]=0.8 Coefficient[43,61]=0.8 Coefficient[43,67]=0.8 Coefficient[49,55]=0.8 Coefficient[49,61]=0.8 Coefficient[49,67]=0.8 Coefficient[55,61]=0.8 Coefficient[55,67]=0.8 Coefficient[61,67]=0.8 Description=0 Coefficient[41,47]=0.8 Coefficient[41,53]=0.8 Coefficient[41,59]=0.8 Coefficient[41,66]=0.8 Coefficient[47,53]=0.8 Coefficient[47,59]=0.8 Coefficient[47,66]=0.8 Coefficient[53,59]=0.8 Coefficient[53,66]=0.8 Coefficient[59,66]=0.8 Coefficient[42,67]=0.8 Coefficient[48,67]=0.8 Coefficient[54,67]=0.8 Coefficient[60,67]=0.8 Coefficient[41,65]=0.8 Coefficient[47,65]=0.8 Coefficient[53,65]=0.8 Coefficient[59,65]=0.8