高效液相色谱法测定制药中间体7-甲氧基-1-萘基乙腈
HPLC Determination of a Pharmaceutical Intermediate-7-Methoxy-1-naphthyl-Acetonitrile
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摘要: 提出了用高效液相色谱法测定制备抗抑药物中间体7-甲氧基-1-萘基乙腈含量的方法.采用Diamonsil-C18色谱柱(250 mm×4.6 mm,5 μm)进行分离,柱温为20 ℃,用甲醇-水(80+20)的混合液为流动相,流量为0.8 mL·min-1,检测波长为231 nm,进样量为20 μL.结果表明:在此色谱条件下,7-甲氧基-1-萘基乙腈与相关杂质得到了分离.7-甲氧基-1-萘基乙腈的质量浓度在2~48 mg·L-1范围内呈线性关系,方法的检出限(3S/N)为105 μg·L-1.在40 mg·L-1浓度水平上平行测定6次,对方法的精密度和回收率做试验,测得其相对标准偏差为0.034%,平均回收率为99.7%.Abstract: HPLC was applied to the determination of 7-methoxy-1-naphthyl-acetonitrile (MONAN),which is an important intermediate in the preparation of anti-depression drugs.The Diamonsil C18 chromatographic column (250 mm×4.6 mm,5 μm) was used as stationary phase for separation of MONAN from co-existing by-products and impurities at column temperature of 20 ℃.A mixture of methanol and H2O (80+20) was used as mobile phase with flow-rate of 0.8 mL·min-1.UV-detection was made at the wavelength of 231 nm.Volume of sample solution introduction was 20 μL.Linear relationship between values of peak area and mass concentration of MONAN was obtained in the range of 2-48 mg·L-1.Detection limit (3S/N) found for the method was 105 μg·L-1.Precision and recovery were tested at the concentration level of 40.0 mg·L-1 of MONAN for 6 determinations,value of RSD and average recovery found were 0.034% and 99.7% respectively.