| 头孢类药物制备过程的HPLC中控分析方法研究 |
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| 引用本文： | 王帅,胡宝祥,程君键,洪黎黎,孙楠. 头孢类药物制备过程的HPLC中控分析方法研究[J]. 浙江化工, 2010, 41(8): 29-31 |
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| 作者姓名： | 王帅 胡宝祥 程君键 洪黎黎 孙楠 |
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| 作者单位： | 1. 浙江工业大学化学工程与材料学院,浙江,杭州,310032
2. 浙江华方药业有限责任公司,浙江,台州,318020 |
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| 基金项目： | 浙江省科技厅科技计划项目:氧头孢烯类抗生素关键中间体的合成 |
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| 摘 要： | 3-乙酰氧基甲基-7β-特丁氧羰基氨基-3-头孢-4-羧酸(3-ATC)是头孢类药物制备的重要中间体,它可通过7-氨基头孢烷酸(7-ACA)和二碳酸二叔丁酯(BOC)反应合成,本文采用高效液相色谱法(HPLC)建立了该反应的中控分析方法。方法采用反相C18色谱柱,以270nm为检测波长,乙腈-离子对试剂(0.01mol/L四丁基溴化铵+0.005mol/L磷酸氢二钠的水溶液,pH7.0)为流动相的条件下分离检测了7-ACA和3-ATC,7-ACA的相对标准偏差、平均回收率、线性范围分别为0.66%(n=5),103.0%(n=3),0.21～2.68×102μg/mL(r=0.9923),3-ATC的相对标准偏差、平均回收率、线性范围分别为0.51%(n=5),99.8%(n=3),0.075～1.06×103μg/mL(r=0.9992)。
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| 关 键 词： | HPLC 7-氨基头孢烷酸 3-乙酰氧基甲基-7β-特丁氧羰基氨基-3-头孢-4-羧酸 |
Control Analysis in Production of Cephalosporin Drugs by HPLC |
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| WANG Shuai,HU Bao-xiang,CHEN Jun-jian,HONG Li-li,SUN Na-na. Control Analysis in Production of Cephalosporin Drugs by HPLC[J]. Zhejiang Chemical Industry, 2010, 41(8): 29-31 |
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| Authors: | WANG Shuai HU Bao-xiang CHEN Jun-jian HONG Li-li SUN Na-na |
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| Affiliation: | WANG Shuai, HU Bao-xiang, CHEN Jun-jian, HONG Li-li, SUN Na-na (1.College of Chemical Engineering and materials science, Zhejiang University of Technology, Hangzhou 310032, China;2.Zhejiang Huafang Pharmaceuticals Co., Ltd., Taizhou 318020, China) |
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| Abstract: | 3-（acetoxymethyl）-7β-（tert-butoxycarbonyl）-8-oxo-5-thia-1-aza-bicyclo [4.2.0]oct-2-ene-2-carboxylic acid （3-ATC）, which was formed by reaction of 7-aminocephaloporinic acid （7-ACA） with di-tert-butyl dicarbonate （BOC）, was an important intermediate for the production of vast cephalosporin drugs.In this work, the reverse phase HPLC was applied to separation and determination of 7-ACA and 3-ATC on a C18 column using 40：60 acetonitrile/ion-pair water solution （0.01mol/L tetrabutylammonium bromide ＋ 0.005mol/L Na2HPO4, pH 7.0） as mobile phase, and UV detector was used at 270 nm wavelength.The RSD, the average recovery and the linear concentration range of 7-ACA were 0.66%（n=5）,103.0%（n=3） and 0.21～2.68×102 μg/mL （r=0.9923）, and of 3-ATC were 0.51%（n=5）, 99.8%（n=3）, 0.075～1.06×103 μg/mL（r=0.9992）. |
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| Keywords: | HPLC |
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