摘要
目的建立超高效液相色谱法(UPLC),通过实验拟定相关测定参数准确检测复方黄连素片中木香烃内酯、去氢木香内酯含量。方法应用UPLC法,自设多组实验参数测定复方黄连素片中木香烃内酯、去氢木香内酯含量,比较试验相关指标及结果的差异性。结果 UPLC测定木香烃内酯和去氢木香内酯线性范围分别为0.0255～0.179μg、0.0266～0.186μg(r>0.999);精密度试验RSD(n=5)分别为0.40%、0.39%(显示精密度良好);稳定性试验RSD(n=4)分别为0.47%、0.36%(显示供试品溶液在24h内稳定);重复性试验RSD分别为0.33%、0.39%(显示研究方法重复性良好);准确度试验平均回收率(n=9)分别为99.4%、99.6%(显示方法准确度良好)。结论 UPLC法测定复方黄连素片中木香烃内酯、去氢木香内酯含量,流动相选择10mmol/L醋酸铵(pH3.5)-乙腈梯度洗脱时基线稳定,漂移和噪音极小。检测波长选择240 nm时检测灵敏度较高。提取溶剂选择三氯甲烷时提取较完全。
Objective To establish the method of accurately measurement the content of costunolide Dehydro- costuslactone in berberine compound Tablets by ultra - high performance liquid chromatography （ UPLC ）. Methods Using UPLC, the assay of costunolide and dehydrocostuslactone in berberine Compound tablets at different experi- ment parameters and conditions, compare the different of relative indexes and results. Results The linear range was 0. 0255 - 0. 179pLg and 0. 0266 - 0. 186 g （ r 〉 0.999 ） for costunolide and dehydrocostuslactone respectively. For costunolide and dehydrocostuslactone, the precision test RSD （ n = 5 ） was 0.40%, 0.39%, indicating good preci- sion;stability test RSD （n = 4）was 0.47 % and 0.36%, indicating that the test solution was stable within 24 hrs;the repeatability RSD were 0.33 % and O. 39%, indicating that the method was reproducibility; the accuracy test aver- age recoveries（ n = 9）were 99.4% ,99.6%, indicating the accuracy of this study. Conclusion For UPLC method,10 mmol / L ammonium acetate （ pH 3.5 ） - acetonitrile gradient elution as mobile phase, the baseline is stable, minimal drift and noise, higher sensitivity detection at wavelength 240 nm, more complete extraction using chloro- form as extraction solvent.
出处
《青海医学院学报》
CAS
2013年第2期117-119,142,共4页
Journal of Qinghai Medical College
关键词
超高效液相色谱法
参数
测定
复方
黄连素
木香烃内酯
去氢木香内酯
Ultra performance liquid chromatography Parameters Determination Berberine Compound Costunolide Dehydrocostuslactone
