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目的:采用气相色谱法测定盐酸金刚乙胺中已知有关物质杂质B、杂质A和杂质C的含量。方法:样品经氢氧化钠碱化处理,正己烷提取,以金刚烷为内标物质,采用分流进样法,以RESTEK Rtx-5毛细管色谱柱(30 m×0.32 mm,0.25μm)为分析柱进行分离测定。结果:杂质A在9.996～199.92μg·ml-1范围内具有良好线性关系(r=0.999 6),平均回收率为98.99%(RSD=0.9%,n=9);杂质B在10.02～200.48μg·ml-1范围内具有良好线性关系(r=0.999 2),平均回收率为99.21%(RSD=0.9%,n=9);杂质C在10.14～202.80μg·ml-1范围内具有良好线性关系(r=0.999 5),平均回收率为100.03%(RSD=1.2%,n=9)。结论:本法灵敏度高、结果准确、重复性好,可用于盐酸金刚乙胺有关物质的测定。
OBJECTIVE: To determine the amount of impurity B, impurity A and impurity C known to rimantadine hydrochloride by gas chromatography. Methods: The sample was alkalized by sodium hydroxide and extracted with n-hexane. Adopting RTAx-5 capillary column (30 m × 0.32 mm, 0.25 μm) as analytical column with adamantane as internal standard, Separation assay. Results: The impurity A showed a good linear relationship (r = 0.999 6) with the average recovery of 98.99% (RSD = 0.9%, n = 9) in the range of 9.996 ~ 199.92μg · ml- (R = 0.999 2), the average recovery was 99.21% (RSD = 0.9%, n = 9). The impurity C had a good linearity in the range of 10.14 ~ 202.80μg · ml-1 (R = 0.999 5). The average recovery was 100.03% (RSD = 1.2%, n = 9). Conclusion: This method has high sensitivity, accurate results and good reproducibility. It can be used for the determination of rimantadine hydrochloride related substances.