伏格列波糖溶出度 JP

2493 Supplement I,JP XVI Official Monographs

Assay Weigh accurately the mass of not less than20Val-

sartan Tablets,and powder.Weigh accurately a portion of the powder,equivalent to about50mg of valsartan (C24H29N5O3),add60mL of the mobile phase,shake thor-oughly,add the mobile phase to make exactly100mL,and centrifuge.Pipet5mL of the supernatant liquid,add exactly 3mL of the internal standard solution,add the mobile phase to make50mL,and use this solution as the sample solution. Separately,weigh accurately about50mg of Valsartan RS (separately,determine the water<2.48>and the residual sol-vent in the same manner as Valsartan),and dissolve in the mobile phase to make exactly100mL.Pipet5mL of this so-lution,add exactly3mL of the internal standard solution, add the mobile phase to make50mL,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 calculate the ratios,Q T and Q S,of the peak area of valsartan to that of the internal standard.

Amount(mg)of valsartan(C24H29N5O3)

＝M S×Q T/Q S

M S:Amount(mg)of Valsartan RS,calculated on the an-hydrous basis and corrected on the amount of the

residual solvent

Internal standard solution—A solution of diclofenac sodium in the mobile phase(1in1000).

Operating conditions—

Detector:An ultraviolet absorption photometer(wave-length:225nm).

Column:A stainless steel column3mm in inside diameter and12.5cm in length,packed with octadecylsilanized silica gel for liquid chromatography(5m m in particle diameter).

Column temperature:A constant temperature of about 259C.

Mobile phase:A mixture of water,acetonitrile,and acetic acid(100)(500:500:1).

Flow rate:Adjust the flow rate so that the retention time of valsartan is about5minutes.

System suitability—

System performance:When the procedure is run with10 m L of the standard solution under the above operating con-ditions,valsartan and the internal standard are eluted in this order with the resolution between these peaks being not less than5.

System repeatability:When the test is repeated6times with10m L of the standard solution under the above operat-ing conditions,the relative standard deviation of the ratio of the peak area of valsartan to that of the internal standard is not more than1.0z.

Containers and storage Containers—Tight containers.Vasopressin Injection

バソプレシン注射液

Change the Assay(ii)as follows:

Assay

(ii)Standard stock solution:Dissolve2000Units of Vasopressin RS,according to the labeled Units,in exactly 100mL of diluted acetic acid(100)(1in400).Pipet1mL of this solution,and add diluted acetic acid(100)(1in400)to make exactly10mL.

Voglibose Tablets

ボグリボース錠

Add the following next to the Uniformity of dosage units:

Dissolution<6.10>When the test is performed at50revolu-tions per minute according to the Paddle method,using900 mL of water as the dissolution medium,the dissolution rate in30minutes of Voglibose Tablets is not less than85z.

Start the test with1tablet of Voglibose Tablets,withdraw not less than20mL of the medium at the specified minute after starting the test,and filter through a membrane filter with a pore size not exceeding0.45m m.Discard the first10 mL of the filtrate,pipet V mL of the subsequent filtrate,add the mobile phase to make exactly V?mL so that each mL contains about0.11m g of voglibose(C10H21NO7),and use this solution as the sample solution.Separately,weigh ac-curately about22mg of voglibose for assay(separately de-termine the water<2.48>in the same manner as Voglibose), and dissolve in water to make exactly100mL.Pipet5mL of this solution,and add water to make exactly100mL.Pipet2 mL of this solution,and add water to make exactly100mL. Pipet10mL of this solution,add the mobile phase to make exactly20mL,and use this solution as the standard solu-tion.Perform the test with exactly100m L each of the sample solution and standard solution as directed under Liquid Chromatography<2.01>according to the following condi-tions,and determine the peak areas,A T and A S,of vogli-bose.

Dissolution rate(z)with respect to the labeled amount of voglibose(C10H21NO7)

＝M S×A T/A S×V?/V×1/C×9/20

M S:Amount(mg)of voglibose for assay

C:Labeled amount(mg)of voglibose(C10H21NO7)in1 tablet

Operating conditions—

Apparatus,detector,column,column temperature,reac-tion coil,cooling coil,reaction reagent,reaction tempera-ture,and flow rate of reaction reagent:Proceed as directed in the operating conditions in the Assay.