【求助】药典中的二种溶出方法
发布于 2011-04-22 · 浏览 2422 · IP 浙江浙江
这个帖子发布于 14 年零 13 天前，其中的信息可能已发生改变或有所发展。
有一点不明白，请大家指教，美国药典32版替扎尼定有两种溶出方法，一种是15min取样，用液相做，一种是30min取样，用紫外做，溶出介质等其他条件一样，我想问的是为啥用二种方法？每批是否要做二种？
先谢了
！
Dissolution
test 1—
Medium: 0.1 N hydrochloric acid; 500 mL, degassed.
Apparatus 1: 100 rpm.
Time: 15 minutes.
Determine the amount of tizanidine (C9H8ClN5S) dissolved by employing the following method.
Phosphoric acid solution, Buffer solution, and Mobile phase— Proceed as directed in the Assay.
Standard stock solution— Dissolve an accurately weighed quantity of USP Tizanidine Hydrochloride RS, and dilute quantitatively, and stepwise if necessary, with Medium to obtain a solution having a concentration of about 201 ?g per mL.
Working standard solution— For Tablets labeled to contain 2 mg, transfer 4.0 mL of the Standard stock solution to a 200-mL volumetric flask, dilute with Medium to volume, and mix. For Tablets labeled to contain 4 mg, transfer 4.0 mL of the Standard stock solution to a 100-mL volumetric flask, dilute with Medium to volume, and mix.
Test solution— Withdraw 10 mL of the solution under test. Pass through a suitable 0.45um filter, discarding the first 5 mL of the filtrate.
Chromatographic system — The liquid chromatograph is equipped with a 230-nm detector and a 4.6-mm × 25-cm column that contains packing L1. The flow rate is about 1.0 mL per minute. The column temperature is maintained at 50. Chromatograph the Working standard solution, and record the peak responses as directed for Procedure: the column efficiency is not less than 2000 theoretical plates; the tailing factor is not more than 2.0; and the relative standard deviation for replicate injections is not more than 2.0%
Tolerances— Not less than 80% (Q) of the labeled amount of C9H8ClN5S is dissolved in 15 minutes.
test 2— If the product complies with this test, the labeling indicates that the product meets USP Dissolution
Test 2.
Medium: 0.1 N hydrochloric acid; 500 mL, deaerated.
Apparatus 1: 100 rpm.
Time: 30 minutes.
Standard solution— Transfer about 23 mg, accurately weighed, of USP Tizanidine Hydrochloride RS to a 250-mL volumetric flask, add about 200 mL of Medium, and sonicate until dissolved. Dilute with Medium to volume. For Tablets labeled to contain 2 mg, transfer 5.0 mL to a 100-mL volumetric flask, and dilute with Medium to volume. For Tablets labeled to contain 4 mg, transfer 10.0 mL to a 100-mL volumetric flask, and dilute with Medium to volume.
Test solution— Pass a portion of the solution under test through a suitable 0.45-?m filter.
Procedure— Determine the amount of tizanidine hydrochloride (C9H8ClN5S·HCl) dissolved by employing UV absorption at the wavelength of maximum absorbance at about 228 nm on the Test solution in comparison with the Standard solution, using a 1.0-cm cell and Medium as the blank. Calculate the percentage of tizanidine dissolved by the formula:
in which AU and AS are the absorbances obtained from the Test solution and Standard solution, respectively; CS is the concentration, in mg per mL, of the Standard solution; 500 is the volume, in mL, of Medium; 100 is the conversion factor to percentage; and L is the Tablet label claim, in mg.
Tolerances— Not less than 80% (Q) of the labeled amount of tizanidine is dissolved in 30 minutes.
先谢了
！
Dissolution
test 1—
Medium: 0.1 N hydrochloric acid; 500 mL, degassed.
Apparatus 1: 100 rpm.
Time: 15 minutes.
Determine the amount of tizanidine (C9H8ClN5S) dissolved by employing the following method.
Phosphoric acid solution, Buffer solution, and Mobile phase— Proceed as directed in the Assay.
Standard stock solution— Dissolve an accurately weighed quantity of USP Tizanidine Hydrochloride RS, and dilute quantitatively, and stepwise if necessary, with Medium to obtain a solution having a concentration of about 201 ?g per mL.
Working standard solution— For Tablets labeled to contain 2 mg, transfer 4.0 mL of the Standard stock solution to a 200-mL volumetric flask, dilute with Medium to volume, and mix. For Tablets labeled to contain 4 mg, transfer 4.0 mL of the Standard stock solution to a 100-mL volumetric flask, dilute with Medium to volume, and mix.
Test solution— Withdraw 10 mL of the solution under test. Pass through a suitable 0.45um filter, discarding the first 5 mL of the filtrate.
Chromatographic system — The liquid chromatograph is equipped with a 230-nm detector and a 4.6-mm × 25-cm column that contains packing L1. The flow rate is about 1.0 mL per minute. The column temperature is maintained at 50. Chromatograph the Working standard solution, and record the peak responses as directed for Procedure: the column efficiency is not less than 2000 theoretical plates; the tailing factor is not more than 2.0; and the relative standard deviation for replicate injections is not more than 2.0%
Tolerances— Not less than 80% (Q) of the labeled amount of C9H8ClN5S is dissolved in 15 minutes.
test 2— If the product complies with this test, the labeling indicates that the product meets USP Dissolution
Test 2.
Medium: 0.1 N hydrochloric acid; 500 mL, deaerated.
Apparatus 1: 100 rpm.
Time: 30 minutes.
Standard solution— Transfer about 23 mg, accurately weighed, of USP Tizanidine Hydrochloride RS to a 250-mL volumetric flask, add about 200 mL of Medium, and sonicate until dissolved. Dilute with Medium to volume. For Tablets labeled to contain 2 mg, transfer 5.0 mL to a 100-mL volumetric flask, and dilute with Medium to volume. For Tablets labeled to contain 4 mg, transfer 10.0 mL to a 100-mL volumetric flask, and dilute with Medium to volume.
Test solution— Pass a portion of the solution under test through a suitable 0.45-?m filter.
Procedure— Determine the amount of tizanidine hydrochloride (C9H8ClN5S·HCl) dissolved by employing UV absorption at the wavelength of maximum absorbance at about 228 nm on the Test solution in comparison with the Standard solution, using a 1.0-cm cell and Medium as the blank. Calculate the percentage of tizanidine dissolved by the formula:
in which AU and AS are the absorbances obtained from the Test solution and Standard solution, respectively; CS is the concentration, in mg per mL, of the Standard solution; 500 is the volume, in mL, of Medium; 100 is the conversion factor to percentage; and L is the Tablet label claim, in mg.
Tolerances— Not less than 80% (Q) of the labeled amount of tizanidine is dissolved in 30 minutes.
最后编辑于 2011-04-22 · 浏览 2422
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