建立了高效液相色谱法测定雷贝拉唑钠原料药中的7 个有关物质。采用C18 色谱柱，以15 mmol/L 磷酸氢二钠溶液( 用磷酸调至pH 6.0) ∶乙腈(60 ∶ 40) 为流动相，检测波长290 nm。雷贝拉唑钠及6 个有关物质均在0.04 ～ 10 μg/ml范围内线性关系良好，另一有关物质2-[(4- 甲氧基-3- 甲基吡啶-2- 基) 甲亚磺酰基]-1H- 苯并咪唑的线性范围为0.04 ～5 μg/ml。7 个有关物质回收率为101.34％～ 107.90％，RSD 为1.00％～ 6.35％。
Abstract
An HPLC method was established for the determination of the related substances in rabeprazole sodium bulk drug. A C18 column was used, with the mobile phase of 15 mmol/L disodium hydrogen phosphate solution (adjusted to pH 6.0 with phosphoric acid)∶acetonitrile (60∶40), at the detection wavelength of 290 nm. The calibration curves of rabeprazole sodium and six related substances were linear in the ranges of 0.04 - 10 μg/ml, while it was linear in the range of 0.04 - 5 μg/ml for 2-[[(4-methoxy-3-methylpyridin-2-yl)methyl]sulfinyl]-1H-benzimidazole. The recoveries for seven related substances were 101.34％ - 107.90％, with RSDs of 1.00％ - 6.35％.
关键词
雷贝拉唑钠 /
有关物质 /
高效液相色谱 /
测定
{{custom_keyword}} /
Key words
rabeprazole sodium /
related substance /
HPLC /
determination
{{custom_keyword}} /
{{custom_sec.title}}
{{custom_sec.title}}
{{custom_sec.content}}
参考文献
[1] Reddy GM, Bhaskar BV, Reddy PP, et al. Identification and characterization of potential impurities of rabeprazole sodium [J]. J Pharm Biomed Anal, 2007, 43(4): 1262-1269.
[2] Vasu Dev R, Sai Uday Kiran G, Venkata Subbaiah B, et al. Identification of degradation products in stressed tablets of rabeprazole sodium by HPLC-hyphenated techniques [J].
Magn Reson Chem, 2009, 47(5): 443-448.
[3] Rao PS, Ray UK, Gupta PB, et al. Identification, isolation and characterization of new impurity in rabeprazole sodium [J]. J Pharm Biomed Anal, 2010, 52(4): 620-624.
[4] Garcia CV, Nudelman NS, Steppe M, et al. Structural elucidation of rabeprazole sodium photodegradation products [J]. J Pharm Biomed Anal, 2008, 46(1): 88-93.
[5] Miura M, Tada H, Satoh S, et al. Determination of rabeprazole enantiomers and their metabolites by high-performance liquid chromatography with solid-phase extraction [J]. J
Pharm Biomed Anal, 2006, 41(2): 565-570.
[6] 孙国祥, 丁 楠, 王 真, 等. HPLC-DAD-MS 鉴定注射用雷贝拉唑钠杂质及其特征谱研究[J]. 沈阳药科大学学报,2011, 28(6): 433-437.
[7] 陈 敖, 王智慧. 雷贝拉唑的合成[J]. 精细与专用化学品,2010, 18(2): 28-29.
[8] 刘 路, 江文明, 任美婷, 等. 雷贝拉唑钠原料药中一未知有关物质的结构解析[ J] . 中国医药工业杂志, 2013,44(12): 1268-1271.
{{custom_fnGroup.title_cn}}
脚注
{{custom_fn.content}}
基金
上海市科学技术委员会项目(11DZ1920907)
{{custom_fund}}
PDF(5319 KB)
