摘要
目的:建立高效液相色谱法测定大鼠肝微粒体中咪达唑仑及1-OH咪达唑仑的含量。方法:色谱柱为COSMOSIL C18柱(4.6 mm×250 mm,5μm),流动相为甲醇∶乙腈∶水(V∶V∶V=55∶11∶34),流速为1.0 ml/min,柱温为25℃,检测波长为220 nm。结果:咪达唑仑和1-OH咪达唑仑线性范围分别是1.0~64.0μm(r=0.999 2)和0.125~8.0μm(r=0.999 4),呈良好的线性关系。咪达唑仑的批内、批间精密度为3.7%~11.2%和4.2%~13.1%,提取回收率为(91.46±9.03)%^(94.54±7.62)%;1-OH咪达唑仑的批内、批间精密度为5.9%~10.4%和7.7%~12.3%,提取回收率为(92.27±8.11)%^(95.16±5.72)%。咪达唑仑和1-OH咪达唑仑在室温保存8 h、反复冻融3次和-20℃保存1周含量稳定,与新鲜样品比较,差异无统计学意义(P>0.05)。结论:本法快速、准确、重现性好,可同时测定大鼠肝微粒体中咪达唑仑及1-OH咪达唑仑的浓度。
OBJECTIVE： To establish a HPLC method for content determination of midazolam and 1-OH midazolam in rat liver mircosome. METHODS： The column was COSMOSIL C18（ 4. 6 mm × 250 mm,5 μm） with the mobile phase of methanol-acetonitrile-water（ V∶ V ∶ V = 55 ∶ 11 ∶ 34） at flow rate of 1. 0 ml / min. The temperature was 25 ℃,and the detection wavelength was at 220 nm. RESULTS： The liner range of midazolam and 1-OH midazolam were respectively1. 0 ~ 64. 0 μm（ r = 0. 999 2） and 0. 125 ~ 8. 0 μm（ r = 0. 999 4）. The RSD range of intra-precision and inter-precision of midazolam were respectively 3. 7% ~ 11. 2% and 4. 2% ~ 13. 1%, and the average extraction recoveries were（ 91. 46 ±9. 03） % ^（ 94. 54 ± 7. 62） %,meanwhile,the RSD range of intra-precision and inter-precision of 1-OH midazolam were respectively 5. 9% ~ 10. 4% and 7. 7% ~ 12. 3%, and the average extraction recoveries were（ 92. 27 ±8. 11） % ^（ 95. 16 ±5. 72） %. The tests for the stability showed that there is no significantly difference between midazolam and 1-OH midazolam during the storage at room temperature for 8 hours,Freeze-thaw cycles for 3 times and stored at- 20 ℃ for 1 week（ P〉 0. 05）. CONCLUSIONS： The method is simple,accurate and repeatable,and can be used for the simultaneous concentration determination of midazolam and 1-OH midazolam in rat liver mircosome.
出处
《中国医院用药评价与分析》
2016年第1期42-45,共4页
Evaluation and Analysis of Drug-use in Hospitals of China
