512JP XV Cilostazol Tablets/O‹cial Monographs
Mobile phase:A mixture of water,acetonitrile and methanol(10:7:3).
Flow rate:Adjust the‰ow rate so that the retention time of cilostazol is about9minutes.
System suitability—
System performance:When the procedure is run with10 m L of the standard solution under the above operating condi-tions,cilostazol and the internal standard are eluted in this order with the resolution between these peaks being not less than9.
System repeatability:When the test is repeated5times with 10m L of the standard solution under the above operating conditions,the relative standard deviation of the ratio of the peak area of cilostazol to that of the internal standard is not more than1.0z.
Containers and storage Containers—Well-closed contain-ers.
Cilostazol Tablets
シロスタゾール錠
Cilostazol Tablets contain not less than95.0z and not more than105.0z of the labeled amount of cilostazol(C20H27N5O2:369.46).
Method of preparation Prepare as directed under Tablets, with Cilostazol.
Identiˆcation Mix well an amount of powdered Cilostazol Tablets,equivalent to50mg of Cilostazol according to the la-beled amount,with10mL of acetone,centrifuge,and use the supernatant liquid as the sample solution.Separately,dis-solve25mg of Cilostazol Reference Standard in5mL of ace-tone,and use this solution as the standard solution.Perform the test with these solutions as directed under Thin-layer Chromatography<2.03>.Spot6m L each of the sample solu-tion and standard solution on a plate of silica gel for thin-lay-er chromatography,develop the plate with a mixture of ethyl acetate,acetonitrile,methanol and formic acid(75:25:5:1)to a distance of about12cm,and air-dry the plate.Spray evenly DragendorŠ's TS for spraying on the plate:the principal spot with the sample solution and the spot with the standard solu-tion are orange in color and have the same R f value. Uniformity of dosage units<6.02>Perform the test accord-ing to the following method:it meets the requirement of the Content uniformity test.
To1tablet of Cilostazol Tablets add2mL of water to dis-integrate the tablet,add the internal standard sol
ution exactly 5mL for a50-mg tablet and exactly10mL for a100-mg tablet,and add methanol to make50mL.Shake for10 minutes for the50-mg tablet and for20minutes for the 100-mg tablet.To1mL of the solution add methanol to make10mL for the50-mg tablet and20mL for the100-mg tablet,ˆlter through a membraneˆlter with pore size of not more than0.5m m,and use theˆltrate as the sample solution. Proceed as directed in the Assay.
Amount(mg)of cilostazol(C20H27N5O2)
＝W S×(Q T/Q S)×(C/50)
W S:Amount(mg)of Cilostazol Reference Standard
C:Labeled amount(mg)of cilostazol(C20H27N5O2)in1 tablet
Internal standard solution—A solution of benzophenone in methanol(1in250).
Dissolution<6.10>Perform the test according to the follow-ing method:it meets the requirement.
Perform the test with1tablet of Cilostazol Tablets at50 revolutions per minute according to the Paddle method,us-ing900mL of a solution of sodium lauryl sulfate(3in1000) as the dissolution medium.Withdra
w20mL or more of the dissolution medium45minutes after starting the test for a 50-mg tablet and60minutes after starting the test for a 100-mg tablet,andˆlter through a membraneˆlter with a pore size not exceeding0.45m m.Discard theˆrst10mL of theˆltrate,pipet the subsequent V mL,add the solution of sodium lauryl sulfate(3in1000)to make exactly V?mL so that each mL contains about5.6m g of cilostazol(C20H27N5 O2)according to the labeled amount,and use this solution as the sample solution.Separately,weigh accurately about28 mg of Cilostazol Reference Standard,previously dried at 1059C for2hours,and dissolve in methanol to make exactly 100mL.Pipet4mL of this solution,add the solution of sodi-um lauryl sulfate(3in1000)to make exactly200mL,and use this solution as the standard solution.Determine the absor-bances,A T and A S,of the sample solution and standard solu-tion at257nm as directed under Ultraviolet-visible Spec-trophotometry using the solution of sodium lauryl sulfate(3 in1000)as the control:the dissolution rates of a50-mg tablet in45minutes and a100-mg tablet in60minutes are not less than75z and not less than70z,respectively.
Dissolution rate(z)with respect to the labeled amount of cilostazol(C20H27N5O2)
＝W S×(A T/A S)×(V?/V)×(1/C)×18
W S:Amount(mg)of Cilostazol Reference Standard
C:Labeled amount(mg)of cilostazol(C20H27N5O2)in1 tablet
Assay Weigh accurately,and powder not less than20 Cilostazol Tablets.Weigh accurately a portion of the pow-der,equivalent to about50mg of cilostazol(C20H27N5O2), add exactly5mL of the internal standard solution and methanol to make50mL,and shake well for10minutes.To 1mL of this solution add methanol to make10mL,ˆlter through a membraneˆlter with a pore size of not more than 0.5m m,and use theˆltrate as the sample solution.Separate-ly,weigh accurately about50mg of Cilostazol Reference Standard,dissolve in a suitable amount of methanol,and add exactly5mL of the internal standard solution and methanol to make50mL.To1mL of this solution add methanol to make10mL,and use this solution as the standard solution. Perform the test with10m L each of the sample solution and standard solution as directed under Liquid Chromatography <2.01>according to the following conditions,and determine the ratios,Q T and Q S,of the peak area of cilostazol to that of the internal standard.
Amount(mg)of cilostazol(C20H27N5O2)
＝W S×(Q T/Q S)
W S:Amount(mg)of Cilostazol Reference Standard Internal standard solution—A solution of benzophenone in methanol(1in250).
513
JP XV
O‹cial Monographs /Cisplatin Operating conditions —
Proceed as directed in the operating conditions in the As-say under Cilostazol.System suitability —
System performance:Proceed as directed in the system suitability in the Assay under Cilostazol.
System repeatability:When the test is repeated 6times with 10m L of the standard solution under the above operating conditions,the relative standard deviation of the ratio of the peak area of cilostazol to that of the internal standard is not more than 1.5z .Containers and storage Containers—Well-closed contain-
ers.
Cimetidine
シメチジン
C 10H 16N 6S:252.34
2-Cyano-1-methyl-3-s 2-[(5-methyl-1H -imidazol-4-yl)methylsulfanyl]ethyl t
guanidine [51481-61-9]Cimetidine,when dried,contains not less than 99.0z of C 10H 16N 6S.
tablet5Description Cimetidine occurs as a white crystalline pow-der.It is odorless,and has a bitter taste.
It is freely soluble in methanol and in acetic acid (100),sparingly soluble in ethanol (95),slightly soluble in water,and practically insoluble in diethyl ether.It dissolves in dilute hydrochloric acid.It is gradually colored by light.Identiˆcation (1)To 0.1mL of a solution of Cimetidine in ethanol (95)(1in 100)add 5mL of citric acid-acetic anhy-dride TS,and heat in a water bath for 15minutes:a red-pur-ple color develops.
(2)Determine the infrared absorption spectrum of Cimetidine,previously dried,as directed in the potassi
um bromide disk method under the Infrared Spectrophotometry <2.25>,and compare the spectrum with the Reference Spec-trum:both spectra exhibit similar intensities of absorption at the same wave numbers.
pH <2.54>Dissolve 0.5g of Cimetidine in 50mL of freshly boiled and cooled water,shake for 5minutes and ˆlter:the pH of the ˆltrate is between 9.0and 10.5.Melting point <2.60>
140–1449C
Purity (1)Clarity and color of solution—Dissolve 1.0g of Cimetidine in 10mL of methanol:the solution is clear and colorless to pale yellow in color.
(2)Heavy metals <1.07>—Proceed with 2.0g of Cimeti-dine according to Method 2,and perform the test.Prepare the control solution with 2.0mL of Standard Lead Solution (not more than 10ppm).
(3)Arsenic <1.11>—Dissolve 1.0g of Cimetidine in 5mL of dilute hydrochloric acid,and perform the test with this so-
lution (not more than 2ppm).
(4)Related substances—Dissolve 0.5g of Cimetidine in 10mL of methanol,and use this solution as the sample solu-tion.Pipet 1mL of the sample solution,add methanol to make exactly 100mL.Pipet 1mL of this solution,add methanol to make exactly 10mL,and use this solution as the standard solution.Perform the test with these solutions as directed under Thin-layer Chromatography <2.03>.Spot 4m L each of the sample solution and standard solution on a plate of silica gel for thin-layer chromatography.Develop the plate with a mixture of ethyl acetate,methanol and ammonia solu-tion (28)(21:2:2)to a distance of about 15cm,air-dry the plate,and then dry at 809C for 30minutes.Allow the plate to stand in iodine vapor for 45minutes:the spots other than the principal spot from the sample solution are not more intense than the spot from the standard solution.Loss on drying <2.41>Not more than 0.5z (1g,1059C,
3hours).
Residue on ignition <2.44>
Not more than 0.2z (1g).
Assay Weigh accurately about 0.24g of Cimetidine,previ-ously dried,dissolve in 75mL of acetic acid (100),and titrate
<2.50>with 0.1mol W L perchloric acid VS (potentiometric titration).Perform a blank determination,and make any necessary correction.
Each mL of 0.1mol W L perchloric acid VS ＝25.23mg of C 10H 16N 6S
Containers and storage Containers—Well-closed contain-ers.
Storage—Light-resistant.
Cisplatin
シスプラチン
Cl 2H 6N 2Pt:300.05
(SP -4-2)-Diamminedichloroplatinum
[15663-27-1]
Cisplatin,when dried,contains not less than 98.0z and not more than 102.0z of Cl 2H 6N 2Pt.
Description Cisplatin occurs as a yellow crystalline powder.It is sparingly soluble in N ,N -dimethylformamide,slightly soluble in water,and practically insoluble in ethanol (99.5).Identiˆcation (1)To 5mL of a solution of Cisplatin (1in 2000)add 2to 3drops of a solution of tin (II)chloride dihydrate (1in 100):a brown precipitate is formed.
(2)Determine the absorption spectrum of a solution of Cisplatin in a solution of sodium chloride in 0.01mol/L hydrochloric acid TS (9in 1000)(1in 2000)as directed under Ultraviolet-visible Spectrophotometry <2.24>,and compare the spectrum with the Reference Spectrum or the spectrum of a solution of Cisplatin Reference Standard prepared in the same manner as the sample solution:both spectra exhibit similar intensities of absorption at the same wavelengths.(3)Determine the infrared absorption spectrum of Cisplatin as directed in the potassium bromide disk method

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