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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 high performance liquid chromatography and micellar electrokinetic capillary chromatography for the determination of nosimazole. Methods: The experimental conditions of HPLC were as follows: Dikma Diamonsil TM (diamond) C 18 column (4.6 mm × 250 mm, 5 μm), acetonitrile-0.05 mol·L -1 (42:58, containing 0.2% triethylamine, pH 3.0) at a flow rate of 1 mL · min -1. The detection wavelength was 278 nm. The injection volume was 20 μL. The column temperature was 30 ℃. The experimental conditions of electrokinetic capillary chromatography were as follows: the column was 68.5 cm × 75 μm and the effective column length was 60 cm. The optimum conditions were 40 mmol·L -1 sodium dihydrogen phosphate and 25 mmol·L ~ 1) SDS (pH 6.0) as electrophoresis medium, operating voltage 25 kV, column temperature: 30 ℃, detection wavelength: 278 nm. Results: This method is simple, sensitive and accurate. The linear range of the two methods was 0.8 ~ 30.0μg · mL ~ (-1) and 27 ~ 269μg · mL ~ (-1) respectively. The regression equation was A = -602.7 + 5 334.0C (r = 0.999 9) and A = 0.007 9 + 0.174C (r = 0.999 7). The average recovery of HPLC was 99.8% (n = 5). Conclusion: The method established in this paper can be used for the determination of nosimazole.