溶出曲线法评价苯磺酸氨氯地平片的质量一致性

目的:建立苯磺酸氨氯地平片体外溶出曲线评价方法,为仿制药一致性评价提供参考。方法:在4种不同介质(水、pH1.2、pH 4.0、pH 6.8)中的溶出度,采用桨板法,转速分别为75转/min和50转/min,HPLC法,在波长237 nm检测。结果:桨板法50转/min区分力好于75转/min,自制品与原研品在四种溶出介质中溶出曲线相似,与体内生物等效试验结果一致。结论:体外溶出曲线法可用于苯磺酸氨氯地平片的仿制药一致性评价。

依折麦布片有关物质的HPLC法测定

建立了高效液相色谱法测定依折麦布片的有关物质。采用Hypersil Gold C8色谱柱,以甲醇∶0.05%三氟乙酸溶液（50∶50）为流动相,检测波长232 nm。依折麦布与其非对映异构体[6,（3R,4S）-1-（4-氟苯基）-3-[（3R）-3-（4-氟苯基）-3-羟基丙基]-4-（4-羟基苯基）-2-氮杂环丁酮]的分离度为1.8;依折麦布及其有关物质2、非对映异构体和有关物质3分别在12~820、9.6~640、12~780和12~780 ng/ml范围内线性关系良好。上述有关物质的相对校正因子分别为0.8、1.0和1.2;平均回收率分别为102.5%、104.4%和97.9%,RSD分别为1.3%、1.7%和2.4%。

Characterization of two degradation products of Azilsartan formed during the micronization process and development of a method to control the degradation

The degradation of Azilsartan in the micronization process was studied and a degradation control method was developed. In the micronization process of Azilsartan, two degradation products （DP-1 and DP-2） were detected by HPLC. DP-1 is a known impurity but DP-2 has not been reported before. The structures of the two degradation products were identified by NMR and MS analysis. The formation of DP- 1 and DP-2 can be controlled by changing the micronization process.

GC-MS法测定左乙拉西坦中的基因毒性杂质4-氯丁酸甲酯和4-氯丁酸乙酯

目的:建立一种气质联用色谱检测左乙拉西坦中基因毒性杂质4-氯丁酸甲酯和4-氯丁酸乙酯含量mL·min-1;进样方式用分流进样,分流比2∶1;载气为氦气;检测器为质谱检测器;离子化方式为EI;溶剂延甲酯和4-氯丁酸乙酯的检测;4-氯丁酸甲酯和4-氯丁酸乙酯在一定范围内线性良好,r均大于0.990 0;定量下限分别为0.979 7、1.789 ng·mL^-1;加样回收率良好,平均加样回收率(n=12)分别为93.9%,90.9%;RSD灵敏度高,专属性和准确度好,可用于左乙拉西坦中4-氯丁酸甲酯和4-氯丁酸乙酯检测。