问题：求美国药典关于盐酸安非他酮的质量标准
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时间：2006-08-30 14:32:39 编辑加入/取消收藏订制/取消短消息举报该贴

求美国药典关于盐酸安非他酮的质量标准．

一定加分

回复人：edwin,★★ (宝剑锋从磨砺出,梅花香自苦寒来) 时间：2006-08-30 14:47:44 编辑

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Bupropion Hydrochloride

C13H18ClNO·HCl 276.21
1-Propanone, 1-(3-chlorophenyl)-2-[(1,1-dimethylethyl)amino]-, hydrochloride, (±)-.
(±)-2-(tert-Butylamino)-3¢-chloropropiophenone hydrochloride [31677-93-7].
» Bupropion Hydrochloride contains not less than 98.0 percent and not more than 102.0 percent of C13H18ClNO·HCl, calculated on the anhydrous basis.
Packaging and storage— Preserve in well-closed, light-resistant containers.
USP Reference standards á11ñ— USP Bupropion Hydrochloride RS. USP Bupropion Hydrochloride Related Compound A RS. USP Bupropion Hydrochloride Related Compound B RS.
Identification—
A: Infrared Absorption á197Kñ.
B: The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that in the chromatogram of the Standard preparation, as obtained in the Assay.
Water, Method I á921ñ: not more than 0.5%.
Chromatographic purity—
TEST 1—
Adsorbent: a 0.25-mm layer of high-performance silica gel, previously washed with methanol.
Test solution— Prepare a solution of Bupropion Hydrochloride in methanol having a concentration of about 100.0 mg per mL.
Standard solutions— Prepare a solution of m-chlorobenzoic acid in methanol containing about 0.5 mg per mL. Dilute this solution quantitatively, and stepwise if necessary, with methanol to obtain solutions having known concentrations of about 0.3, 0.2, and 0.1 mg per mL.
Application volume: 2 µL.
Developing solvent system: a mixture of toluene, cyclohexane, and glacial acetic acid (47:47:6).
Procedure— Proceed as directed for Thin-Layer Chromatography under Chromatography á621ñ. Locate and quantitate the spots obtained by scanning the entire plate with a suitable densitometer at 254 nm. Plot a standard curve of area versus concentrations of the Standard solutions. From the standard curve, determine the percentages of m-chlorobenzoic acid and any other impurity present: not more than 0.2% of m-chlorobenzoic acid is found; and not more than 0.1% of any other individual impurity is found.
TEST 2—
Procedure— Using the chromatograms obtained in the Assay, calculate the percentage of each impurity in the portion of Bupropion Hydrochloride taken by the formula:
100F(ri / rS),
in which F is the relative response factor for each impurity (see the accompanying table for values); ri is the peak response for each impurity obtained from the Assay preparation; and rS is the peak response for bupropion hydrochloride obtained from the Standard preparation. The limits of impurities are specified in the accompanying table: not more than 0.3% of total unidentified impurities is found; and not more than 1.0% of total impurities is found, the results of Test 1 and Test 2 being added.

Relative retention time Relative response factor (F) Limit (%)
0.38 0.68 0.5
0.58 0.96 0.2
0.71 2.22 0.1
0.78 0.82 0.1
0.92 0.73 0.2
1.14 — 0.2a
1.63 1.13 0.1
2.30 0.91 0.2
2.74 1.45 0.2
all other peaksb 1.00 0.1
a The percentage is determined by direct comparison to the area of the peak for bupropion hydrochloride related compound B obtained from the System suitability solution.
b Except the peaks with relative retention time of 1.14.

Content of chloride— Dissolve about 50.0 mg of Bupropion Hydrochloride, accurately weighed, in 50 mL of water, and titrate with 0.1 N silver nitrate VS, determining the endpoint potentiometrically. Perform a blank determination, and make any necessary corrections. Each mL of 0.1 N silver nitrate is equivalent to 3.545 mg of chloride (Cl): not less than 12.6% and not more than 13.1% of chloride, calculated on the anhydrous basis, is found.
Assay—
Diluent— Prepare a mixture of methanol and water (1:1).
0.025 M Phosphate buffer— Dissolve 6.8 g of monobasic potassium phosphate in about 1900 mL of water. Adjust with 1 N sodium hydroxide to a pH of 7.0, dilute with water to 2000 mL, and mix.
Mobile phase— Prepare a filtered and degassed mixture of 0.025 M Phosphate buffer, methanol, and tetrahydrofuran (51:39:11). Make adjustments if necessary (see System Suitability under Chromatography á621ñ).
System suitability solution— Dissolve accurately weighed quantities of USP Bupropion Hydrochloride Related Compound A RS and USP Bupropion Hydrochloride Related Compound B RS in Diluent to obtain a solution having known concentrations of about 0.025 mg of each per mL.
Standard preparation— Transfer 25 mg of USP Bupropion Hydrochloride RS, accurately weighed, to a 25-mL volumetric flask. Dissolve in a portion of Diluent, pipet 2.0 mL of the System suitability solution into the flask, dilute with Diluent to volume, and mix.
Assay preparation— Transfer about 50 mg of Bupropion Hydrochloride, accurately weighed, to a 50-mL volumetric flask, dissolve in and dilute with Diluent to volume, and mix.
Chromatographic system (see Chromatography á621ñ)— The liquid chromatograph is equipped with a 250-nm detector and a 3.9-mm × 15-cm column that contains 5-µm packing L7. The flow rate is about 1.1 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the relative retention times are about 0.92 for bupropion hydrochloride related compound A and 1.14 for bupropion hydrochloride related compound B; the resolution, R, between bupropion hydrochloride related compound A and bupropion hydrochloride is not less than 1.3; and the relative standard deviation for replicate injections is not more than 2.0% determined from bupropion hydrochloride and not more than 5.0% determined from bupropion hydrochloride related compound B.
Procedure— Separately inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the areas for the major peaks. Calculate the quantity, in mg, of C13H18ClNO·HCl in the portion of Bupropion Hydrochloride taken by the formula:
50C(rU / rS),
in which C is the concentration, in mg per mL, of USP Bupropion Hydrochloride RS in the Standard preparation; and rU and rS are the peak responses obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information— Staff Liaison : Salvador C. Salado, M.S., Scientist and Latin American Liaison
Expert Committee : (PA3) Pharmaceutical Analysis 3
USP28–NF23 Page 296
Pharmacopeial Forum : Volume No. 29(4) Page 1011
Phone Number : 1-301-816-8165

回复人：mqx110,▲ (-) 时间：2006-08-30 14:54:03 编辑	2楼
谢谢了

得分人：edwin-1,

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