摘要
建立了高效液相色谱(HPLC)法和胶束电动毛细管色谱(MECC)法测定盐酸去甲万古霉素中去甲万古霉素的含量。色谱条件HPLCKromasilC18柱;流动相A0.3mol/L甲酸铵溶液(pH7.5)-水(15∶85),B0.3mol/L甲酸铵溶液(pH7.5)-二氧六环(15∶85);梯度洗脱;柱温35℃;检测波长280nm;MECC熔融石英毛细管柱;背景电解质含0.06mol/L十六烷基三甲基溴化铵的0.12mol/L三羟甲基氨基甲烷-磷酸盐缓冲液(pH3.0);外加电压-15kV;柱温25℃;检测波长220nm。采用本文的HPLC和MECC方法,去甲万古霉素与有关物质尤其是与主要杂质之间的分离较好。HPLC方法和中国药典方法对暂行国家标准品和2批供试品中去甲万古霉素含量的测定结果一致。由于此前在标定暂行标准品时所用色谱系统未能分离出主要未知杂质,因而标准品的去甲万古霉素含量的标示值明显偏高,且测定结果揭示该批标准品中去甲万古霉素的含量显著低于中国药典的规定,故建议有关部门制备新的盐酸去甲万古霉素国家标准品。
An high performance liquid chromatography (HPLC) method and a micellar electrokinetic capillary chromatography (MECC) method for determination of the content of norvancomycin (NV), the primary component in NV hydrochloride, were established. The chromatographic conditions were as follows: HPLC: Kromasil C 18 column; mobile phase: A: 0 3mol/L ammonium formate (pH7 5)-water (15∶85), B: 0 3mol/L ammonium formate(pH7 5)-dioxane (15∶85); gradient elution; column temperature: 35℃; detection wavelength: 280nm; MECC: bare fused silica capillary; background electrolyte: 0 12 mol/L tris (hydroxymethyl) aminomethane phosphate buffer (pH3 0) containing 0 06mol/L cetyltrimethylammonium bromide; applied voltage: -15kV; capillary temperature: 25℃; detection wavelength: 220nm. The proposed HPLC method and MECC method allow good separation of NV from its related substances, which is much better than that obtained with the existing methods. The two methods showed better selectivity and high efficiency than the method of current Chinese Pharmacopoeia (ChP), especially towards a primary unknown impurity which was now baseline separated from NV. There was good agreement between the proposed HPLC method and the method of ChP for determination of the content of NV in NV hydrochloride and its pharmaceutical preparations. Since the primary unknown impurity was not separated under the conditions of the method of ChP during the preparation of the temporary national standard fifteen years ago, and the results indicated that the content of NV in this batch of standard did not complied with the requirement of ChP. It is recommended that a new national standard be prepared.
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2004年第10期592-597,共6页
Chinese Journal of Antibiotics
关键词
盐酸去甲万古霉素
去甲万古霉素含量
有关物质
高效液相色谱
胶束电动毛细管色谱
Norvancomycin hydrochloride
Content of norvancomycin
Related substances
High performance liquid chromatography
Micellar electrokinetic capillary chromatography
