高效液相色谱法测定尼莫地平及制剂中光降解产物的含量

Determination of light-introduced degradation products in nimodipine and preparations by HPLC

目的：建立尼莫地平及制剂中光降解产物含量的测定方法。方法：采用反相高效液相色谱法，Shiseido CAPCELL PAK C18（250mm×4．6mm，5μm）色谱柱，流动相为甲醇-乙腈-水（35：38：27），流速为1．0ml／min，检测波长为235nm。结果：尼莫地平和杂质A在0．1—4μg／ml的浓度范围内，均与其峰面积呈良好线性（尼莫地平：r=0．999996，n=6；杂质A：r=0．999995，n=6）。精密度试验尼莫地平的RSD为0．1％（n=5），杂质A的RSD为1．2％（n=5），尼莫地平的最低检测限为0．02ng，杂质A的定量限为0．2ng。结论：本方法简便、结果准确，能控制尼莫地平及其制剂的质量。

Objective ： To establish HPLC method for determining the light - introduced degradation products in nimodipine and its preparations. Method： Shiseido CAPCELL PAK C18 （ 250 mm × 4.6 mm,5 μm ） column was applied as stationary phase and methanol- acetonitrile- water（ 35： 38： 27） acted as mobile phase,the flow rate of which was 1.0 ml/min. The detection wavelength was at 235 nm. Results ： The assay exhibited a good linearity over the concentration range of 0.1 - 4 μg/ml （ nimodipine ： r = 0. 999 996, n = 6 ; impurity A ： r = 0. 999 995, n = 6 ）. RSD for nimodipine was 0.1% （ n = 5 ）, and 1.2% （ n = 5 ） for impurity A. The limit of detection （ LOD ）of nimodipine was 0.02 ng, and the limit of quantitativity （ LOQ ） of impurity A was 0.2 ng. Conclusion ： The method established in this paper is simple, accurate, and has provided the good guarantee for quality control of nimodipine and its preparations.