HPLC法测定阿托伐他汀钙3种中间体的含量和有关物质_张明颖.pdfVIP

HPLC 法测定阿托伐他汀钙3种中间体的含量和有关物质 ＊ # 张明颖 ，孙国祥（沈阳药科大学药学院，沈阳 110016） 中图分类号 R927.2 文献标志码 A 文章编号 1001-0408（2013）01-0083-03 DOI 10.6039/j.issn. 1001-0408.2013.01.30 摘 要 目的：建立测定阿托伐他汀钙3种中间体的含量和有关物质的方法。方法：采用高效液相色谱法。3种中间体4- 氟苯基 苄基酮（FPAP ）、苯基戊酰胺类化合物（M-2）和乙酸叔丁酯类化合物（L- 1）分别使用乙腈-四氢呋喃-50mmol/L 枸橼酸铵溶液（pH 4.0，3∶2∶5）、甲醇-50mmol/L 磷酸二氢钠溶液（60∶40）和甲醇-水（85∶15）为流动相；FPAP 以Agilent Eclipse XDB-C18柱分析，M-2 和L- 1以Century SIL C18 BDS 柱分析；流速均为1.0ml/min ；柱温为（30±0.15）℃；检测波长均为244nm ；进样量为20μl。结果： FPAP 、M-2和L- 1检测质量浓度线性范围分别为5～100、5～150、5～150μg/ml（r ＝0.9999～1.0000），平均回收率分别为99.27％、 99.43％、99.97％，RSD 分别为0.07％、0.37％、0.11％；FPAP 、M-2、L- 13种中间体的含量应分别不低于98％、98％、99％，有关物质 应分别小于0.5％、1％、0.5％。结论：所建立的方法简单、准确、重复性好，可用于阿托伐他汀钙3种中间体的质量控制。 关键词 HPLC 法；阿托伐他汀钙；中间体；含量测定；有关物质 Content Determination and Related Substances of 3Kinds of Intermediates of Atorvastatin Calcium by HPLC ZHANG Ming-ying ，SUN Guo-xiang （College of Pharmacy ，Shenyang Pharmaceutical University ，Shenyang 110016，China ） ABSTRACT OBJECTIVE ：To establish the method for content determination and related substances of 3intermediates of atorvas- tatin calcium. METHODS ：HPLC method was adopted. 3 Intermediates including 4-fluoro-2-phenylacetophenone （FPAP ），phenyl pentanamide compound （M-2），and tertiary butyl acteate compound （L- 1）. The separation of FPAP was performed on Agilent Eclipse XDB-C18 column with acetonitrile-tetrahydrofuran-50 mmol/L ammonium citrate （pH ＝4.0，3∶2∶5）as the mobile phase. The separation of M-2 and L-1were performed on Century SIL C18 BDS column with mobile phase consisted of methanol-50mmol/ L sodium dihydrogen phosphate （60∶40）for M-2 and methanol-water （85∶15）for L-1. The flow rate was 1.0ml/min ，and column temperature was set at （30±0.15）℃. The detection wavelengths were set at 244 nm and injection volume was 20 μl. RESULTS ： The linear ranges were 5-100μg/ml for FPAP ，5-150μg/ml for M-2，and 5-1