摘要
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：Established a reversed-phase HPLC method for the determination of three impurities in nitrazepam and its tablets firstly.Method：The separation was performed on a Venusil XBP C8（250 mm×4.6 mm,5 μm） column.The mobile phase consisted of 20 mmol·L-1 potassium dihydrogen phosphate solution-methanol-trehydrofuran （40：48：12）,the flow rate was 1.0 mL·min-1,the column temperature was 30 ℃.The detection wavelength was set at 220 nm.The injection volume was 10 μL.Results：A good separation for nitrazepam and three impurities was achieved.The linear ranges of impurities A,B and C were 0.27-15.90 μg·mL-1（r=0.9999）,0.25-14.85 μg·mL-1（r=0.9998） and 0.26-15.40 μg·mL-1（r=0.9997）,respectively.The average recoveries of impurities A,B and C at three levels were 101.2% （RSD：1.9%）,99.8% （RSD：1.2%） and 101.3% （RSD：1.3%）,respectively.The LDLs were 0.27 ng,0.25 ng and 0.26 ng,respectively.Conclusion：The established HPLC method can quantity three impurities in nitrazepam and its tablets simultaneously and accurately.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2010年第8期1477-1481,共5页
Chinese Journal of Pharmaceutical Analysis
基金
"十一五"国家科技支撑计划重点项目子课题"苯二氮类药品安全控制检验技术研究"(2008BAI55B05-001)
