| 查看: 1259 | 回复: 3 | |||
[求助]
求助USP36 利培酮片含量、有关物质的检测方法
|
| 利培酮片 Risperidone Tablets！谁可以提供帮助，谢谢大家了！！ |
回复此楼» 猜你喜欢
酯类化合物柱层析极性较大，使用醇类溶剂，怎么避免酯交换
已经有3人回复
-
求助骆广生微化工技术书籍
已经有1人回复
-
药物学论文润色/翻译怎么收费?
已经有105人回复
-
求助冯连芳、张才亮的《聚合过程强化技术》
已经有1人回复
-
求助Isoeugenol质量标准
已经有0人回复
-
Gliclazide
已经有0人回复
-
塞替派/噻替哌（Thiotepa） 质量控制
已经有15人回复
-
2026考博
已经有0人回复
-
有没有大佬可以帮忙查下Trijardy XR和Qternmet XR历年销售数据呀
已经有0人回复
-
浙江中医药大学张勇民院士2026年博士研究生招生
已经有3人回复
-
硫醚氧化
已经有2人回复
» 本主题相关价值贴推荐，对您同样有帮助:
- 【求助】有关醇胺类物质浓度的检测方法
已经有3人回复
- 【求助】门冬氨酸鸟氨酸有关物质检测方法
已经有16人回复
kobeyy
金虫 (正式写手)
- 应助: 7 (幼儿园)
- 金币: 3346.6
- 散金: 5
- 红花: 4
- 帖子: 436
- 在线: 203.8小时
- 虫号: 341450
- 注册: 2007-04-08
- 性别: GG
- 专业: 色谱分析
【答案】应助回帖
★
感谢参与，应助指数 +1
yuanahen: 金币+1, 感谢参与，应该有所帮助 2013-06-03 12:30:32
感谢参与，应助指数 +1
yuanahen: 金币+1, 感谢参与，应该有所帮助 2013-06-03 12:30:32
|
Risperidone Tablets Risperidone Tablets contain not less than 90.0 percent and not more than 110.0 percent of the labeled amount of risperidone (C23H27FN4O2). Packaging and storage?? Preserve in tight, light-resistant containers. Store at controlled room temperature. USP Reference standards 11?? USP Risperidone RS 3-[2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidino]ethyl]-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one [CAS-106266-06-2].410.48 Identification?? A: Infrared Absorption?? Test solution?? Grind an appropriate number of Tablets to prepare a 550 ?? 50 ?? per mL solution of risperidone in ethyl acetate. Shake the solution for 30 minutes, and centrifuge for 20 minutes. Evaporate 5 mL of the supernatant with the aid of a stream of nitrogen to 2 mL on a warm water bath. Add 150 ?? 50 mg of KBr powder, mix well, and evaporate to dryness. Grind the dried mixture, and press a small amount into a transparent pellet 197K. Standard solution?? Grind about 2 mg of USP Risperidone RS with about 200 mg of KBr powder, and press into a transparent pellet. 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. Dissolution 711?? Medium: 0.1 N hydrochloric acid; 500 mL. Apparatus 2: 50 rpm. Time: 45 minutes. Determine the amount of C23H27FN4O2 dissolved by employing the following method. Mobile phase?? Prepare a filtered and degassed mixture of water and acetonitrile (65:35), and add 1 mL of trifluoroacetic acid to each 1 L of the mixture. Adjust with ammonium hydroxide to a pH of 3.0. Make adjustments if necessary (see System Suitability under Chromatography 621). Standard solution?? Dissolve an accurately weighed quantity of USP Risperidone RS in Medium, and dilute quantitatively, and stepwise if necessary, with Medium to obtain a solution having a known concentration of about 0.006 mg per mL. Test solution?? Use portions of the solution under test, and pass through a suitable filter having a porosity of 35 ??. Chromatographic system (see Chromatography 621)?? The liquid chromatograph is equipped with a 237-nm detector and a 4.6-mm ?? 15-cm column that contains 5-?? packing L1. The flow rate is about 1.5 mL per minute. Chromatograph the Standard solution and the Test solution as directed for Procedure: the retention time of risperidone is about 2.1 minutes, and the relative standard deviation for replicate injections is not more than 2.0%. Procedure?? Separately inject equal volumes (about 50 L) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the peak responses. Calculate the percentage of C23H27FN4O2 dissolved by the formula: in which rU and rS are the peak responses obtained from the Test solution and the Standard solution, respectively; CS is the concentration, in mg per mL, of USP Risperidone RS in 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 75% (Q) of the labeled amount of C23H27FN4O2 is dissolved in 45 minutes. Uniformity of dosage units 905?? Mobile phase and Chromatographic system?? Proceed as directed for Dissolution. Standard solution?? Dissolve an accurately weighed quantity of USP Risperidone RS in a suitable volumetric flask, and dilute quantitatively with 0.1 N hydrochloric acid to obtain a solution having a known concentration of about 0.03 mg of risperidone per mL. Test solution?? Transfer one Tablet into a 100-mL volumetric flask, add 50 mL of 0.1 N hydrochloric acid, and shake mechanically for about 30 minutes. Dilute with 0.1 N hydrochloric acid to volume, and mix. Pass a portion of this solution through a suitable filter having a 0.2-?? or finer porosity, and use the filtrate. Procedure?? Separately inject equal volumes (about 20 L) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the areas for the risperidone peak. Calculate the quantitiy, in mg, of risperidone (C23H27FN4O2) in the portion of Tablets taken by the formula: C(rU /rS)100 in which C is the concentration, in mg per mL, of USP Risperidone RS in the Standard solution; and rU and rS are the peak responses obtained from the Test solution and the Standard solution, respectively. Related compounds?? Mobile phase and Diluent?? Proceed as directed in the Assay. Standard solution?? Prepare as directed for the Standard preparation in the Assay. Diluted sodium hydroxide?? To 1 L of water in a beaker, add 0.1 N sodium hydroxide dropwise to obtain a pH of about 8.5. Diluted hydrogen peroxide?? Dilute 1 mL of hydrogen peroxide with water to 500 mL. Peak identification solution?? Suspend 10 mg of USP Risperidone RS in 10 mL of Diluted sodium hydroxide in a 100-mL volumetric flask. Store the flask at 90 for 24 hours. Cool the solution to room temperature. Add 10 mL of aqueous Diluted hydrogen peroxide to the flask, and store at 90 for an additional two hours. Cool the mixture to room temperature, and dilute with methanol to volume. Test solution?? Use the Assay preparation. Chromatographic system (see Chromatography 621)?? Proceed as directed in the Assay. Chromatograph about 20 L of the Peak identification solution, record the peak responses as directed for Procedure, and identify the peaks using the relative retention times given in Table 1: the resolution, R, between the trans-N-oxide and cis-N-oxide is not less than 1.2. [note??The approximate relative retention times given in Table 1 are for identification purposes only. ] Table 1 Peak Identfication Approximate Relative Retention Time (RRT) Relative Response Factor (R) Limit of Impurity Bicyclorisperidone1 0.68 0.81 Not more than 0.5% Risperidone 1.0 1.0 ?? Risperidone trans-N-oxide2 1.65 ?? Not quantified. Used for identification and system suitability check only. Risperidone cis-N-oxide3 1.81 0.95 Not more than 0.5% Any other unspecified degradation product ?? 1.0 Not more than 0.3% Total impurities ?? ?? Not more than 1.0% 1 3-(4-fluoro-2-hydroxyphenyl)-1-[2-(6,7,8,9-tetrahydro-2-methyl-4-oxo-4H-pyrido-[1,2-a]pyrimidin-3-yl)ethyl]-2-aza-1-azoniabicyclo[2.2.2]oct-2-ene iodide. 2 trans-3-[2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl]-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one, N-oxide monohydrate. 3 cis-3-[2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl]-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one, N-oxide monohydrate. Procedure?? Inject a volume (about 20 L) of the Test solution into the chromatograph, record the chromatogram, and measure the responses for all of the peaks. Calculate the percentage of each impurity in the portion of Tablets taken by the formula: 100(1/R)(ri /rS) in which R is the appropriate relative response factor as listed in Table 1; ri is the peak response for each impurity in the Test solution; and rS is the peak response of risperidone in the Test solution: not more than 0.3% of any individual unidentified impurity is found, not more than 0.5% of any individual specified impurity is found, and not more than 1.0% of total impurities is found. Assay?? Diluent?? Prepare a degassed mixture of methanol and water (80:20). Solution A?? Prepare a filtered and degassed mixture of water, acetonitrile, and trifluroacetic acid (80:19.5:0.1). Adjust with ammonium hydroxide to a pH of 3.0. Solution B?? Prepare a filtered and degassed mixture of water, methanol, and trifluoroacetic acid (61:39:0.1). Adjust with ammonium hydroxide to a pH of 3.0. Mobile phase?? Use variable mixtures of Solution A and Solution B as directed for Chromatographic system. Make adjustments if necessary (see System Suitability under Chromatography 621). Standard preparation?? Transfer an accurately weighed quantity of USP Risperidone RS to a suitable volumetric flask, and dissolve in and dilute quantitatively with Diluent to obtain a solution having a known concentration of about 0.1 mg per mL. Assay preparation?? Transfer an accurately weighed portion of not fewer than 10 Tablets to a volumetric flask that can accommodate a final concentration of 0.1 mg of risperidone per mL. Add an appropriate amount of water equivalent to 20% of the total volume of the volumetric flask, and mechanically shake for about 30 minutes. Add a volume of methanol equivalent to 60% of the total volume of the volumetric flask, and mechanically shake for about 30 minutes. Dilute with methanol to volume, and mix to obtain the final 0.1 mg per mL concentration. Pass a portion of this solution through a suitable filter having a 0.45-?? or finer porosity, and use the filtrate. Chromatographic system (see Chromatography 621)?? The liquid chromatograph is equipped with a 275-nm detector and a 4.6-mm ?? 15-cm column that contains 5-?? packing L1. The flow rate is about 2.5 mL per minute. The column is maintained at room temperature. The chromatograph is programmed as follows. Time (minutes) Solution A (%) Solution B (%) Elution 0?C8 100 0 isocratic 8?C16 100?? 0100 linear gradient 16?C20 0 100 isocratic 20?C21 0100 100?? linear gradient 21?C30 100 0 re-equilbration Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the tailing factor of risperidone is not more than 2.5; and the relative standard deviation for replicate injections is not more than 2.0%. Procedure?? Separately inject equal volumes (about 20 L) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the risperidone peak. Calculate the quantity, in mg, of risperidone (C23H27FN4O2) in the portion of Tablets taken by the formula: 100(CS /CU)(rU / rS) in which CS is the concentration, in mg per mL, of USP Risperidone RS in the Standard preparation; CU is the concentration, in mg per mL, of risperidone in the Assay preparation; and rU and rS are the peak responses of risperidone obtained from the Assay preparation and the Standard preparation, respectively. Auxiliary Information?? Please check for your question in the FAQs before contacting USP. Topic/Question Contact Expert Committee Monograph Ravi Ravichandran, Ph.D. Principal Scientific Liaison 1-301-816-8330 (SM42010) Monographs - Small Molecules 4 Reference Standards RS Technical Services 1-301-816-8129 rstech@usp.org 711 Margareth R.C. Marques, Ph.D. Senior Scientific Liaison 1-301-816-8106 (GCDF2010) General Chapters - Dosage Forms USP36?CNF31 Page 5065 Pharmacopeial Forum: Volume No. 32(4) Page 1109 Chromatographic Column?? RISPERIDONE TABLETS Chromatographic columns text is not derived from, and not part of, USP 36 or NF 31. |
2楼2013-06-03 12:11:11
kobeyy
金虫 (正式写手)
- 应助: 7 (幼儿园)
- 金币: 3346.6
- 散金: 5
- 红花: 4
- 帖子: 436
- 在线: 203.8小时
- 虫号: 341450
- 注册: 2007-04-08
- 性别: GG
- 专业: 色谱分析
3楼2013-06-03 12:11:54
4楼2013-06-05 10:01:45