高效液相色谱法测定盐酸赛庚啶的有关物质

Assay of cyproheptadine hydrochloride and the related substances with HPLC

目的建立测定盐酸赛庚啶有关物质的高效液相色谱法。方法选用Agilent Eclipse XDB-C18柱(4.6mm×250mm,5μm);流动相:乙腈-缓冲液[称取辛烷磺酸钠2.16g,加水约500ml,溶解,加入冰醋酸10.0ml和三乙胺5.0ml,加水至1 000ml,摇匀,用三乙胺调节pH至7.0](85∶15,V/V),过滤并脱气;流速:1.0ml/min;检测波长:286nm;进样量:10μl;柱温:25℃。结果盐酸赛庚啶和杂质A、B、C的线性范围分别为0.056 2~5.620μg/ml(r=0.999 8),0.052 4~5.240μg/ml(r=1.000 0),0.050 3~5.032μg/ml(r=0.999 9),0.053 2~5.316μg/ml(r=0.999 7);盐酸赛庚啶和杂质A、B、C的定量限在0.049~0.054μg/m1之间,检测限在0.019~0.022μg/ml之间;回收率在98%~100%之间;重复性RSD为5.5%(n=6)。结论该方法简便灵敏,结果准确可靠,重复性好,可用于盐酸赛庚啶有关物质的质量控制。

Objective To establish a HPLC method for the assay of cyproheptadine hydrochloride and the related substances. Methods The HPLC was performed on an Agilent Eclipse XDB- C18 column （4.6 mm × 250 mm, 5 μm） at the temper ature of 25 ℃ with the mobile phase of acetonitrile-buffer Solution （ Dissolve 2. 16 g of sodium octane-1-sulfonate with about 500 ml of water and mix well. Add 10. 0 ml of glacial acetic acid and 5. 0 ml of triethylamine, and dilute with water to 1 000 ml, mix well and adiust to pH 7.0 with triethylamine） （85 ： 15,V/V）. The flow rate was 1.0 ml/min and detection wavelength was 286 nm. The injection volume was 10 μl. Results The calibration curves of cyproheptadine hydrochloride, impurityA, Band C showed good linear response in the range from 0. 056 2 to 5. 620 gg/ml （r=0. 999 8）, 0. 052 4 to 5. 240 gg/ml（r=1. 000 0）,0. 050 3 to 5. 032 μg/ml （r=0. 999 9） and 0. 053 2 to 5. 316 μg/ml（r=0. 999 8） respectively. The LOQs for cyproheptadine hydroehloride, impurity A, B and C were within 0. 049-0. 054 μg/ml, LODs were within 0. 019- 0. 022 μg/ml with recovery between 98%-100%. RSD of repeatability was 5.5% （n= 6）. Conclusion This method gave an accurate and reliable results. It can be used for quality control of eyproheptadine hydrochloride.