 |
 |
 |
 |
 |
 |
||
 |
 |
 |
 |
 |
| 4 | 1/1 | 返回列表 |
| 查看: 1312 | 回復(fù): 3 | ||
[求助]
求助USP36 利培酮片含量、有關(guān)物質(zhì)的檢測方法
|
| 利培酮片 Risperidone Tablets！誰可以提供幫助，謝謝大家了��！ |
回復(fù)此樓» 猜你喜歡
是否屬于脾腎陽虛證
已經(jīng)有0人回復(fù)
-
CSC改派-博士生交流訪學(xué)
已經(jīng)有19人回復(fù)
-
藥物學(xué)論文潤色/翻譯怎么收費(fèi)?
已經(jīng)有161人回復(fù)
-
中山大學(xué)-第七醫(yī)院-招科研助理1名（基因設(shè)計(jì)和克隆、RNA合成）
已經(jīng)有0人回復(fù)
-
中山大學(xué)-第七醫(yī)院-招科研助理1名（基因設(shè)計(jì)和克隆、RNA合成）
已經(jīng)有1人回復(fù)
-
巴黎薩克雷大學(xué)與國家留學(xué)基金委合作博士研究生項(xiàng)目-脂質(zhì)納米藥物/生物材料/多酚遞送
已經(jīng)有10人回復(fù)
-
廣西醫(yī)科大學(xué)基礎(chǔ)醫(yī)學(xué)院自身免疫病課題組招收基礎(chǔ)醫(yī)學(xué)相關(guān)專業(yè)的調(diào)劑研究生
已經(jīng)有2人回復(fù)
-
錦州醫(yī)科大學(xué)藥用生物材料（專業(yè)代碼1007Z1）招收調(diào)劑考生
已經(jīng)有0人回復(fù)
-
錦州醫(yī)科大學(xué)藥用生物材料（專業(yè)代碼1007Z1）招收調(diào)劑考生
已經(jīng)有1人回復(fù)
-
26申博自薦
已經(jīng)有6人回復(fù)
» 本主題相關(guān)價(jià)值貼推薦，對您同樣有幫助:
- 【求助】有關(guān)醇胺類物質(zhì)濃度的檢測方法
已經(jīng)有3人回復(fù)
- 【求助】門冬氨酸鳥氨酸有關(guān)物質(zhì)檢測方法
已經(jīng)有16人回復(fù)
kobeyy
金蟲 (正式寫手)
- 應(yīng)助: 7 (幼兒園)
- 金幣: 3346.6
- 散金: 5
- 紅花: 4
- 帖子: 436
- 在線: 203.8小時(shí)
- 蟲號: 341450
- 注冊: 2007-04-08
- 性別: GG
- 專業(yè): 色譜分析
【答案】應(yīng)助回帖
★
感謝參與，應(yīng)助指數(shù) +1
yuanahen: 金幣+1, 感謝參與，應(yīng)該有所幫助 2013-06-03 12:30:32
感謝參與，應(yīng)助指數(shù) +1
yuanahen: 金幣+1, 感謝參與，應(yīng)該有所幫助 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樓2013-06-03 12:11:11
kobeyy
金蟲 (正式寫手)
- 應(yīng)助: 7 (幼兒園)
- 金幣: 3346.6
- 散金: 5
- 紅花: 4
- 帖子: 436
- 在線: 203.8小時(shí)
- 蟲號: 341450
- 注冊: 2007-04-08
- 性別: GG
- 專業(yè): 色譜分析
3樓2013-06-03 12:11:54
4樓2013-06-05 10:01:45
相關(guān)版塊跳轉(zhuǎn)
我要訂閱樓主 bangzi85 的主題更新
| 4 | 1/1 | 返回列表 |
| 最具人氣熱帖推薦 [查看全部] | 作者 | 回/看 | 最后發(fā)表 | |
|---|---|---|---|---|
|
[考研] 材料與化工085600，總分304，本科有兩篇sci參與，求調(diào)劑 +4 | 幸運(yùn)的醬醬 2026-03-22 | 5/250 |
|
|---|---|---|---|---|
|
[考研] 一志愿武理材料工程348求調(diào)劑 +5 | ￣^￣゜汗 2026-03-19 | 7/350 |
|
|
|
[考研] 311求調(diào)劑 +3 | 26研0 2026-03-20 | 3/150 |
|
|
|
[考研] 318求調(diào)劑 +4 | plum李子 2026-03-21 | 7/350 |
|
|
|
[考研] 一志愿華中科技大學(xué)071000，求調(diào)劑 +4 | 沿岸有貝殼6 2026-03-21 | 4/200 |
|
|
|
[考研] 資源與環(huán)境 調(diào)劑申請(333分) +5 | holy J 2026-03-21 | 5/250 |
|
|
|
[考研] 326求調(diào)劑 +5 | 諾貝爾化學(xué)獎(jiǎng)覬?/a> 2026-03-15 | 8/400 |
|
|
|
[考研] 297求調(diào)劑 +3 | 喜歡還是不甘心 2026-03-20 | 3/150 |
|
|
|
[考研] 求調(diào)劑 +3 | .m.. 2026-03-21 | 4/200 |
|
|
|
[考研] 求調(diào)劑 +3 | 白QF 2026-03-21 | 3/150 |
|
|
|
[考研] 332求調(diào)劑 +3 | 鳳凰院丁真 2026-03-20 | 3/150 |
|
|
|
[考研] 301求調(diào)劑 +10 | yy要上岸呀 2026-03-17 | 10/500 |
|
|
|
[考研] 083200學(xué)碩321分一志愿暨南大學(xué)求調(diào)劑 +3 | innocenceF 2026-03-17 | 3/150 |
|
|
|
[考研] 一志愿華中科技大學(xué)，080502，354分求調(diào)劑 +5 | 守候夕陽CF 2026-03-18 | 5/250 |
|
|
|
[考研] 321求調(diào)劑 +9 | 何潤采123 2026-03-18 | 11/550 |
|
|
|
[考研] 求調(diào)劑一志愿南京航空航天大學(xué)289分 +3 | @taotao 2026-03-19 | 3/150 |
|
|
|
[考研] 一志愿 南京航空航天大學(xué)大學(xué) ，080500材料科學(xué)與工程學(xué)碩 +5 | @taotao 2026-03-20 | 5/250 |
|
|
|
[考研] 085410人工智能專碩317求調(diào)劑（0854都可以） +4 | xbxudjdn 2026-03-18 | 4/200 |
|
|
|
[考研] 277調(diào)劑 +5 | 自由煎餅果子 2026-03-16 | 6/300 |
|
|
|
[考研] 一志愿蘇州大學(xué)材料工程（085601）專碩有科研經(jīng)歷三項(xiàng)國獎(jiǎng)兩個(gè)實(shí)用型專利一項(xiàng)省級立項(xiàng) +6 | 大火山小火山 2026-03-16 | 8/400 |
|