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目的:建立反相HPLC同时测定硝西泮原料及片剂中3种杂质的方法。方法:采用Venusil XBPC8柱(250mm×4.6mm,5μm),以20mmol·L-1的磷酸二氢钾水溶液-甲醇-四氢呋喃(40∶48∶12)为流动相,流速1.0mL.min-1,检测波长220nm,柱温30℃;进样量10μL。结果:硝西泮与各杂质峰均能良好的分离。杂质A、B、C分别在0.27～15.90μg·mL-1,0.25～14.85μg·mL-1,0.26～15.40μg·mL-1浓度范围内峰面积与浓度成良好的线性关系;高、中、低3个浓度的平均回收率分别为101.2%(RSD为1.9%),99.8%(RSD为1.2%),101.3%(RSD为1.3%);最低检测限分别为0.27,0.25,0.26ng。结论:该方法简便、灵敏,专属性好,可同时测定硝西泮原料和片剂中3种杂质的量。
Objective: To establish a method for simultaneous determination of three impurities in raw materials and tablets of nitrazepam by reverse phase HPLC. Methods: Venusil XBPC8 column (250 mm × 4.6 mm, 5 μm) was used with a mobile phase of 20 mmol·L -1 potassium dihydrogen phosphate in methanol-tetrahydrofuran (40:48:12) at a flow rate of 1.0 mL · min -1. Detection wavelength 220nm, column temperature 30 ℃; injection volume 10μL. Results: Nitrazepam and impurity peaks were well separated. The peak areas and the concentrations of impurities A, B and C in the range of 0.27 ~ 15.90μg · mL-1, 0.25 ~ 14.85μg · mL-1 and 0.26 ~ 15.40μg · mL- The average recoveries of the three concentrations were 101.2% (RSD 1.9%), 99.8% (RSD 1.2%) and 101.3% (RSD 1.3%). The minimum detection limits were 0.27,0.25,0.26ng. Conclusion: The method is simple, sensitive and specific. It can simultaneously determine the amount of three impurities in raw materials and tablets of nitrazepam.