诺司咪唑含量测定方法的探讨

Study on the Determination of Norastemizole

目的:建立了测定诺司咪唑含量的高效液相色谱法和胶束电动毛细管色谱法。方法:高效液相色谱法的实验条件:选用Dikma Diamonsil^(TM)(钻石)C_(18)色谱柱(4.6 mm×250 mm,5μm),乙腈-0.05mol·L^(-1)磷酸二氢钠水溶液(42:58,含0.2％三乙胺,pH 3.0),流速:1mL·min^(-1),检测波长:278 nm;进样量:20μL;柱温:30℃;胶束电动毛细管色谱法的实验条件:采用石英毛细管柱(未涂层)68.5 cm×75μm,有效柱长60 cm,优化选择40 mmol·L^(-1)磷酸二氢钠+25mmol·L^(-1)SDS(pH 6.0)为电泳介质,操作电压25 kV,柱温:30℃,检测波长:278 nm。结果:本法简便、灵敏、准确。两法线性范围分别为:0.8～30.0μg·mL^(-1)和27～269 μg·mL^(-1),回归方程分别为A=-602.7+5 334.0C(r=0.999 9)和A=0.007 9+0.174C(r=0.999 7),高效液相色谱法的平均回收率为99.8％(n=5)。结论:本文建立的方法可用于诺司咪唑的含量测定。

Objective: To establish a HPLC and MEKC method to determine the content of norastemizole. Method: The HPLC system consisted of Dikma DiamonsilTM C18 column (4.6 mm × 250 mm, 5μm) , acetonitrile -0.05 mol· L-1 NaH2PO4 (42:58, contained 0.2% triethyl amine, pH 3.0), flow rate was 1mL· min-1 and detected with UV at 278 nm, the injection volume was 20 μL, column temperature was 30℃ ; The MEKC experimental conditions were as follows, the electrophoretic medium was composed of 40 mmol · L-1 NaH2PO4 and 25 mmol · L-1 SDS ( pH 6. 0) , uncoated capillary was used (68. 5 cm × 75μm) and detected with UV at 278 nm. The experimental voltage was 25 kV and the separation temperature was 30℃ . Results: Those methods were simple, sensitive and accurate. The linear ranges of HPLC method and MEKC method were 0. 8 - 30. 0μg· mL-1 and 27 - 269 μg· mL-1 ; regression equations were A = -602. 7+5 334. 0C (r =0.999 9) and A = 0. 007 9 + 0. 174C (r =0. 999 7) respectively. For HPLC method, the average recovery of norastemizole was 99. 8% ( n = 5). Conclusion: Those methods could be used for the determination of norastemizole.