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【助已完结】头孢克肟颗粒质量标准
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各位大哥，大姐：谁有头孢克肟颗粒的最新质量标准！！！ 多谢了！！！ [ Last edited by junjun517 on 2010-1-29 at 15:36 ] |
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★ ★
junjun517(金币+2):谢谢参与 2010-01-29 11:12
junjun517(金币+2):谢谢参与 2010-01-29 11:12
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头孢克肟颗粒 Toubaokewo Keli Cefixime Granules 本品含头孢克肟（C16H15N5O7S2）应为标示量的90.0％～110.0%。 【性状】 本品为混悬颗粒。 【鉴别】 (1) 取本品，加磷酸盐缓冲液(pH7.0)制成每1ml中约含10g的溶液，滤过，取续滤液，照紫外－可见分光光度法（附录Ⅳ A）测定，在288nm波长处有最大吸收。 (2) 在含量测定项下记录的色谱图中，供试品溶液主峰的保留时间应与对照品溶液主峰的保留时间一致。 【检查】 酸度 取本品，加水制成1ml含头孢克肟1mg的混悬液，依法测定（附录Ⅵ H），pH值应为2.5～4.5。 水分 取本品，照水分测定法（附录Ⅷ M第一法A）测定，含水分不得过2.0％。 溶出度 取本品，照溶出度测定法（附录X C第二法），以磷酸盐缓冲液（pH7.2）[取6.8g磷酸二氢钾，用适量水溶解，用1mol/L的氢氧化钠溶液调节pH值至7.2，用水稀释至1000ml。]900ml为溶出介质，转速为每分钟50转，依法操作。经30分钟时，取溶液适量，滤过，精密量取续滤液适量，用溶出介质定量稀释制成每1ml中约含头孢克肟10mg的溶液，照紫外－可见分光光度法（附录Ⅳ A），在288nm波长处测定吸光度；另精密称取头孢克肟对照品适量，用溶出介质溶解并定量稀释制成每1ml中约含10mg的溶液（必要时先用少量甲醇溶解，甲醇量不得超过对照品溶液总体积的0.1%），同法测定。计算每包的溶出量。限度为标示量的80%，应符合规定。 有关物质 取本品装量差异项下的内容物适量（约相当于头孢克肟0.1g），置100ml量瓶中，用磷酸盐缓冲液（pH7.0）溶解并稀释至刻度，摇匀，滤过，取续滤液作为供试品溶液；照头孢克肟项下的方法测定，单个杂质峰的峰面积不得大于对照溶液的主峰面积（1.0％），各杂质峰面积的和不得大于对照溶液主峰面积的6倍（6.0％）。 其他 应符合颗粒剂项下有关的各项规定（附录I N）。 【含量测定】取本品装量差异项下的内容物适量（约相当于头孢克肟50mg），精密称定，置250ml量瓶中，用流动相溶解并稀释至刻度，摇匀，滤过，取续滤液l，照头孢克肟项下的方法测定，即得。 【类别】同头孢克肟 【规格】50mg ( 按C16H15N5O7S2计算) 【贮藏】遮光，密封，在阴凉处保存。 附: 微生物限度 照微生物限度检查法（附录XI J）测定。取供试品10g，加pH7.0无菌氯化钠-蛋白胨缓冲液（45℃）100ml置匀浆罐，匀浆2分钟（3000转/分钟），制成1:10的溶液。将1:10的溶液离心5分钟（500转/分钟），上清液为1:10的供试液。按常规法，取1:10的供试液1ml，测定真菌数；按薄膜过滤法，取1:10的供试液1ml，加入0.1%蛋白胨水100ml（45℃）中，全量通过薄膜后，冲洗3次（100ml/次），取出滤膜贴至含2mlβ-内酰胺酶的营养琼脂平板，测定细菌数；按薄膜过滤法，取1:10的供试液10ml，加入0.1%蛋白胨水100ml（45℃）中，全量通过薄膜后，冲洗3次（100ml/次），取出滤膜接种至含2mlβ-内酰胺酶的胆盐乳糖增菌培养基（100ml/瓶）中，检查控制菌。 |
13楼2010-01-29 09:38:16
帮顶一下， |
2楼2010-01-28 09:38:19
★ ★ ★
小木虫(金币+0.5):给个红包，谢谢回帖交流
junjun517(金币+2):谢谢回帖交流 2010-01-28 16:18
小木虫(金币+0.5):给个红包，谢谢回帖交流
junjun517(金币+2):谢谢回帖交流 2010-01-28 16:18
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Re:,头孢克肟质量标准 盐酸头孢吡肟 |ggtb\W Cefepime Hydrochloride REcKfJTj qfAnMBM1@ C19H25ClN6O5S2 ·HCl· H2O 571.50 S H" » Cefepime Hydrochloride contains the equivalent of not less than 825 µg and not more than 911 µg of cefepime (C19H24N6O5S2 ) per mg, calculated on the anhydrous basis. n0K+/}m Packaging and storage— Preserve in tight, light-resistant containers, and store at controlled room temperature. ,' Labeling— Where it is intended for use in preparing injectable dosage forms, the label states that it is sterile or must be subjected to further processing during the preparation of injectable dosage forms. I"8Z'<|/\q USP Reference standards 11 — USP Cefepime Hydrochloride RS. USP Cefepime Hydrochloride System Suitability RS. USP Endotoxin RS. fS8Pi,! Identification, Infrared Absorption 197M . Qi qRx Test specimen— Proceed as directed in the chapter, but do not dry. c8_,S[W Crystallinity 695 : meets the requirements. E+ XR [p Bacterial endotoxins 85 — Where the label states that Cefepime Hydrochloride is sterile or that it must be subjected to further processing during the preparation of injectable dosage forms, it contains not more than 0.04 USP Endotoxin Unit per mg of cefepime hydrochloride. V sL*&Fk Water, Method I 921 : between 3.0% and 4.5%. E=bZ4 / Residue on ignition 281 : not more than 0.1%. 8@6*d.+e Heavy metals, Method II 231 : 0.002%. PKGqu,J, Limit of N -methylpyrrolidine— dry%a T Mobile phase— Prepare a filtered and degassed mixture of 0.01 N nitric acid and acetonitrile (100:1). Make adjustments if necessary (see System Suitability under Chromatography 621 ). y#O/Xw Standard solution— Transfer about 0.16 mL of N-methylpyrrolidine, accurately weighed, to a 100-mL volumetric flask, dissolve in and dilute with water to volume, and mix. Transfer 4.0 mL of this solution to a 100-mL volumetric flask, dilute with 0.01 N nitric acid to volume, and mix. This solution contains about 0.05 mg of N-methylpyrrolidine per mL. '81R wp Test solution— Transfer about 100 mg of Cefepime Hydrochloride, accurately weighed, to a 10-mL volumetric flask, dissolve in and dilute with 0.01 N nitric acid to volume, and mix. [ NOTE— Use this solution within 30 minutes. ] &Ci_wDJ Chromatographic system (see Chromatography 621 )— The liquid chromatograph is equipped with a conductivity detector and a 4.6-mm × 5-cm column that contains 5-µm packing L52. The flow rate is about 1 mL per minute. Chromatograph the Standard solution, and record the peak responses as directed for Procedure: the retention time of N-methylpyrrolidine is not less than 8 minutes, and the relative standard deviation for replicate injections is not more than 5.0%. LG?b]'# Procedure— Separately inject equal volumes (about 100 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms, and measure the peak responses for N-methylpyrrolidine. Calculate the percentage of N-methylpyrrolidine in the portion of Cefepime Hydrochloride taken by the formula: S;{[]; 1000(C/W)( r U / r S), On@p5YRwW in which C is the concentration, in mg per mL, of N-methylpyrrolidine in the Standard solution; W is the quantity, in mg, of Cefepime Hydrochloride taken to prepare the Test solution; and r U and r S are the N-methylpyrrolidine peak responses obtained from the Test solution and the Standard solution, respectively: not more than 0.3% is found. `ih#>i_ & Related compounds— s6oIj$ Potassium phosphate solution— Dissolve 0.68 g of monobasic potassium phosphate in 1000 mL of water. NE@P8pQ> Solution A— Prepare a mixture of Potassium phosphate solution and acetonitrile (9:1). Adjust with a potassium hydroxide solution (2 in 100) to a pH of 5.0, filter, and degas. tqU8>d0^ Solution B— Prepare a mixture of Potassium phosphate solution and acetonitrile (1:1). Adjust with a potassium hydroxide solution (2 in 100) to a pH of 5.0, filter, and degas. d5=yAn-+= 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 ). fydQaxCN D System suitability solution— Prepare a solution of USP Cefepime Hydrochloride System Suitability RS in Solution A containing about 1.4 mg per mL. 9kas]zQ%=P Test solution— Transfer about 70 mg of Cefepime Hydrochloride, accurately weighed, to a 50-mL volumetric flask, dissolve in and dilute with Solution A to volume, sonicate, and mix. [ NOTE— Inject this solution immediately, or store in a refrigerator and inject within 12 hours. ] S ^@# %> Chromatographic system (see Chromatography 621 )— The liquid chromatograph is equipped with a 254-nm detector and a 4.6-mm × 25-cm column that contains 5-µm packing L1. The flow rate is about 1 mL per minute. The chromatograph is programmed as follows. I#CS;Yh95 Time -k3WY&9, (minutes) Solution A Eqt>_n8 (%) Solution B :,MI,SwnS (%) Elution toC|vn&P 0–10 100 0 isocratic Qk g([q4 10–30 100®50 0®50 linear gradient wRE2rsXoU 30–35 50 50 isocratic \'Ca%j 35–36 50®100 50®0 linear gradient 'J#uD|9) %967#XI[y Chromatograph the System suitability solution, and record the peak responses as directed for Procedure: the relative retention times are about 2.7 for cefepime related compound A, 4.3 for cefepime related compound B, and 1.0 for cefepime; and the resolution, R, between cefepime and cefepime related compound A is not less than 5 and between cefepime related compound A and cefepime related compound B is not less than 10. Chromatograph the Test solution, and record the peak responses as directed for Procedure: the capacity factor, k¢, is more than 0.6; the column efficiency is not less than 4000 theoretical plates; and the tailing factor is not more than 1.1. 6T A2 Procedure— Inject a volume (about 10 µL) of the Test solution into the chromatograph, record the chromatogram, and measure the peak responses. Calculate the percentage of each impurity in the portion of Cefepime Hydrochloride taken by the formula: 0XrOOYmx 100( r i / r s ), H6-{(: *< in which r i is the peak response for each impurity; and r s is the sum of the responses for all the peaks: not more than 0.3% of cefepime related compound A is found; not more than 0.2% of cefepime related compound B is found; and not more than 0.1% of any other impurity is found. =`BPGfC b Residual solvents 467 : meets the requirements. I K Dh)Zm (Official January 1, 2007) "0l7%@z*)q Other requirements— Where the label states that Cefepime Hydrochloride is sterile, it meets the requirements for Sterility under Cefepime for Injection. l j*J|%~ Assay— [=I==?2`X Mobile phase— Dissolve 5.76 g of sodium 1-pentanesulfonate in 2000 mL of water. Adjust with glacial acetic acid to a pH of 3.4, and then with potassium hydroxide TS to a pH of 4.0. Prepare a filtered and degassed mixture of this solution and acetonitrile (94:6). Make adjustments if necessary (see System Suitability under Chromatography 621 ). q5(Z Standard preparation— Dissolve an accurately weighed quantity of USP Cefepime Hydrochloride RS in Mobile phase to obtain a solution having a known concentration of about 1.4 mg per mL. r<L>~S>yb Assay preparation— Transfer about 70 mg of Cefepime Hydrochloride, accurately weighed, to a 50-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix. 2VNfnk Chromatographic system (see Chromatography 621 )— The liquid chromatograph is equipped with a 254-nm detector and a 3.9-mm × 30-cm column that contains packing L1. The flow rate is about 2 mL per minute. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the column efficiency is not less than 1500 theoretical plates; the tailing factor is not more than 1.7; and the relative standard deviation for replicate injections is not more than 2.0%. .Qeml4(`3 Procedure— Separately inject equal volumes (about 10 µL) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the quantity, in µg, of cefepime (C19H24N6O5S2 ) in each mg of Cefepime Hydrochloride taken by the formula: g?caE) 50(CP/W)( r U / r S ), -'!%\E;5 in which C is the concentration, in mg per mL, of USP Cefepime Hydrochloride RS in the Standard preparation; P is the content, in µg per mg, of cefepime in USP Cefepime Hydrochloride RS; W is the weight, in mg, of Cefepime Hydrochloride taken to prepare the Assay preparation; and r U and r S are the peak responses obtained from the Assay preparation and the Standard preparation, respectively. i\?P> Auxiliary Information— Staff Liaison : Brian D. Gilbert, Ph.D., Scientist UPkD^D, Expert Committee : (MDANT05) Monograph Development-Antibiotics <KDl2>O USP29–NF24 Page 409 J12 ZdC'O Pharmacopeial Forum : Volume No. 29(5) Page 1437 zSi SZMP" Phone Number : 1-301-816-8223 |
4楼2010-01-28 15:26:25
5楼2010-01-28 15:27:31