Assay of cyproheptadine hydrochloride and the related substances with HPLC
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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。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.
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Key words:
- cyproheptadine hydrochloride /
- related substances /
- HPLC
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