| 高效液相色谱法测定盐酸赛庚啶的有关物质 |
| 投稿时间：2016-09-03 修订日期：2016-10-14 点此下载全文 |
| 引用本文：吴荷琴,陈朝霞.高效液相色谱法测定盐酸赛庚啶的有关物质[J].药学实践杂志,2017,35(1):60~63,69 |
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| 中文摘要: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（4.6 mm×250 mm，5 μm）；流动相：乙腈-缓冲液[称取辛烷磺酸钠2.16 g，加水约500 ml，溶解，加入冰醋酸10.0 ml和三乙胺5.0 ml，加水至1 000 ml，摇匀，用三乙胺调节pH至7.0]（85：15，V/V），过滤并脱气；流速：1.0 ml/min；检测波长：286 nm；进样量：10 μl；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 2~5.620 μg/ml（r=0.999 8），0.052 4~5.240 μg/ml（r=1.000 0），0.050 3~5.032 μg/ml（r=0.999 9），0.053 2~5.316 μg/ml（r=0.999 7）；盐酸赛庚啶和杂质A、B、C的定量限在0.049~0.054 μg/m1之间，检测限在0.019~0.022 μg/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。 |
| 中文关键词:盐酸赛庚啶 有关物质 高效液相色谱法 |
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| Assay of cyproheptadine hydrochloride and the related substances with HPLC |
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| Abstract: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 temperature 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 adjust 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, impurity A, B and C showed good linear response in the range from 0.056 2 to 5.620 μg/ml (r=0.999 8), 0.052 4 to 5.240 μg/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 hydrochloride, 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 cyproheptadine hydrochloride. |
| keywords:cyproheptadine hydrochloride related substances HPLC |
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