盐酸倍他司汀片有关物质检测方法研究
发布时间:2019-01-09 14:15
【摘要】:目的:建立测定盐酸倍他司汀片中乙烯吡啶、2-羟乙基吡啶、N-甲基-2吡啶乙胺等有关物质的检查方法。方法:采用高效液相色谱法,以十八烷基硅烷键合硅胶为填充剂,以缓冲液(称取醋酸铵0.69 g,用1 000 m L水溶解,以冰醋酸调节p H至4.7后,再加4.43 g十二烷基硫酸钠溶解,脱气)-乙腈(60∶40)为流动相,流速1.0 m L·min-1,检测波长259 nm,柱温40℃。结果:各杂质与主成分能完全分离,乙烯吡啶、2-羟乙基吡啶、N-甲基-2吡啶乙胺最低检测限(S/N=3)分别为0.4、0.4、4 ng,回收率分别为97.9%、98.1%、101.7%,浓度与峰面积均呈线性(r0.999)。4个生产企业119批样品检验,共检出已知杂质2个(2-羟乙基吡啶、N-甲基-2吡啶乙胺)及未知杂质6个,各批次间检查的杂质个数及杂质量不同:2-羟乙基吡啶、N-甲基-2吡啶乙胺含量分别为0.005%~0.47%、0.040%~1.26%,总杂质量在0.2%~5.3%范围内。结论:本文建立的方法符合方法学验证要求,可用于盐酸倍他司汀有关物质检查。根据样品检测结果,建议将总杂质量定为2%。
[Abstract]:Objective: to establish a method for the determination of ethylpyridine, 2-hydroxyethylpyridine, N-methyl-2-pyridylethylamine and other related substances in Betastine Hydrochloride tablets. Methods: high performance liquid chromatography (HPLC) with octadecyl silane bonded silica gel as filler, buffer solution (ammonium acetate 0.69 g, dissolved in water of 1 000 mL), and acetic acid (acetic acid) were used to regulate pH to 4.7. The mobile phase was composed of 4.43 g sodium dodecyl sulfate dissolved and degassed) -acetonitrile (60:40). The flow rate was 1.0 mL min-1, and the column temperature was 40 鈩,
本文编号:2405735
[Abstract]:Objective: to establish a method for the determination of ethylpyridine, 2-hydroxyethylpyridine, N-methyl-2-pyridylethylamine and other related substances in Betastine Hydrochloride tablets. Methods: high performance liquid chromatography (HPLC) with octadecyl silane bonded silica gel as filler, buffer solution (ammonium acetate 0.69 g, dissolved in water of 1 000 mL), and acetic acid (acetic acid) were used to regulate pH to 4.7. The mobile phase was composed of 4.43 g sodium dodecyl sulfate dissolved and degassed) -acetonitrile (60:40). The flow rate was 1.0 mL min-1, and the column temperature was 40 鈩,
本文编号:2405735
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