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| 1 | 氟康唑杂质H国家标准物质的研制显示文摘目的以氟康唑杂质H为例,介绍氟康唑系列杂质标准物质研制过程,同时揭示杂质标准物质研制过程中的一些特殊问题。方法第一采用质谱、红外和核磁方法对该杂质进行结构确证,第二采用《欧洲药典》8. 0版和《中国药典》2010年版二部氟康唑有关物质检查方法测定原料的纯度,采用LC-MS等方法对2个液相色谱系统产生的主要杂质进行分析,并测定了氟康唑杂质H的水分和炽灼残渣,第三采用核磁定量方法确定了氟康唑杂质的含量。结果氟康唑杂质H与《欧洲药典》8. 0版中规定的结构一致。水分含量0. 05%,无机杂质含量0. 04%,HPLC有关物质测定过程中发现氟康唑杂质H在水溶液中会部分降解为杂质G,有关物质不能准确测定。核磁方法测定氟康唑杂质H含量为99. 5%。结论由于氟康唑杂质H本身结构的特点,使得常规的质量平衡法不适合为该杂质赋值,定量核磁共振法成为为标准物质定值的有力补充方法。 | 冯艳春 王晨 田冶 常祎卓 马步芳 姚尚辰 胡昌勤 | 2018 | 中国药学杂志2018，53，17： | 5 |
| 2 | HPLC法测定氟康唑的有关物质及最大未知杂质结构鉴定显示文摘目的:建立HPLC法测定氟康唑的有关物质,并对最大未知杂质进行结构鉴定。方法:采用CERI L-column ODS(250 mm×4.6 mm,5μm)色谱柱,以0.01 mol·L^(-1)醋酸钠缓冲液(pH 5.0)-甲醇(95∶5)为流动相A,乙腈-甲醇(60∶40)为流动相B,梯度洗脱,流速1.0 m L·min^(-1),检测波长261 nm,柱温30℃。用LC-MS分析最大未知杂质,再用半制备液相色谱分离纯化,通过NMR确定结构。结果:建立的HPLC有关物质分析方法具有良好的方法学验证结果,与中国药典方法比较,杂质检出能力更强;最大未知杂质为2-(2,4-二氟苯基)^(-1),3-二(1H^(-1),2,4-三唑^(-1)-基)-丁-2-醇。结论:建立的方法简便、灵敏,专属性好,杂质检出能力强,能有效地反应药品质量。 | 王成刚 刘照振 王亚男 李文东 王俊秋 马一星 | 2016 | 药物分析杂志2016，36，7： | 4 |
| 3 | Irbesartan desmotropes:Solid-state characterization,thermodynamic study and dissolution properties显示文摘Irbesartan (IBS) is a tetrazole derivative and antihypertensive drug that has two interconvertible structures, 1H- and 2H-tautomers. The difference between them lies in the protonation of the tetrazole ring. In the solid-state, both tautomers can be isolated as crystal forms A (1H-tautomer) and B (2H-tautomer). Studies have reported that IBS is a polymorphic system and its forms A and B are related monotropically. These reports indicate form B as the most stable and less soluble form. Therefore, the goal of this contribution is to demonstrate through a complete solid-state characterization, thermodynamic study and dissolution properties that the IBS forms are desmotropes that are not related monotropically. However, the intention is also to call attention to the importance of conducting strict chemical and in solid-state quality controls on the IBS raw materials. Hence, powder X-ray diffraction (PXRD) and Raman spectroscopy (RS) at ambient and non-ambient conditions, differential scanning calorimetry (DSC), hot stage microscopy (HSM), Fourier transform infrared (FT-IR) and scanning electron microscopy (SEM) techniques were applied. Furthermore, intrinsic dissolution rate (IDR) and structural stability studies at 98% relative humidity (RH), 25℃ and 40 ℃ were conducted as well. The results show that in fact, form A is approximately four-fold more soluble than form B. In addition, both IBS forms are stable at ambient conditions. Nevertheless, structural and/or chemical instability was observed in form B at 40℃ and 98% RH. IBS has been confirmed as a desmotropic system rather than a polymorphic one. Consequently, forms A and B are not related monotropically. | Andrea Mariela Araya-Sibaja Carlos Eduardo Maduro de Campos Cinira Fandaruff Jose Roberto Vega-Baudrit Teodolito Guillen-Giron Mirtha Navarro-Hoyos Silvia Lucía Cuffini | 2019 | Journal of Pharmaceutical Analysis2019，9，5： | 0 |
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