目的:建立高效液相色谱-二极管阵列检测-质谱法(HPLC-DAD-MS)同时测定藏药花锚中6个[口山]酮类成分,即5个[口山]酮苷元,1-羟基-2,3,5-三甲氧基-[口山]酮(HM-1),1-羟基-2,3,4,7-四甲氧基-[口山]酮(HM-2),1-羟基-2,3,4,5-四甲氧基-[口山]酮(HM-3),1,7-二羟基2,3,4,5-四甲氧基-[口山]酮(HM-4),1,5-二羟基-2,3-二甲氧基-[口山]酮(HM-5)及1个[口山]酮苷,1-O-[β-D-木糖-(1-6)-β-D-葡糖]-2,3,5-三甲氧基-[口山]酮(HM-2-10)的含量。方法:采用Alltima C18色谱柱(4.6mm×250mm,5μm),以乙腈-0.5%醋酸(v/v)进行梯度洗脱(0mim,20:80;20min,70:30;30min,80:20;30.1min,20:80;35min,20:80),流速0.8mL·min^-1,检测波长252nm,离子源APCI,扫描模式正离子。结果:HM-1、HM-2、HM-3、HM-4、HM-5和HM-2-10分别在0.05-5.0,0.05-5.0,0.05-5.0,0.05-10.0,0.05-5.0,0.05-2.0,0.05-2.0μg的范围内线性关系良好(r分别为0.9999,0.9999,0.9997,0.9999,0.9999,0.9992);HM-1、HM-2和HM-3平均回收率(n=9)分别为95.20%,99.80%,97.37%。结论:本法简便、准确,重现性好,可作为藏药花锚药材质量检测的方法。
Objective:To develop a high performance liquid chromatography -diode array detection - mass spec- trometry ( HPLC - DAD - MS)method for simultaneous determination of six major xanthones (five xanthone aglycons and one xanthone glycoside)present in a Tibetan herb,Halenia elliptica. Methods:The analysis was achieved on an Alltima C l8 column (4.6mm×250mm ,5μm)using a mobile phase of acetonitrile -0. 5 % acetic acid gradient elution in a total run time of 35 min(0 min ,20:80 ;20 min,70:30 ;30 min ,80:20 ;30. 1 min ,20:80 ;35 min, 20: 80) and a diode array detector was set at 252 nm. The Agilent 1100 LC/MSD Trap system was equipped with an APCI source using a positive ionization mode. Results: HM - 1, HM - 2, HM - 3, HM - 4, HM - 5, and HM - 2 - 10 were linear over the range of 0.05 - 5.0,0. 05 - 5.0,0.05 - 5.0,0. 05 - 1.00,0.05 - 5.0,0. 05 - 2. 0,0. 05 - 2.0μg ( r was 0.9999,0.9999, 0.9997, 0.9999, 0.9999, 0. 9992, respectively ). The average recoveries ( n = 9 ) were 95.20% ,99.80% ,97.37% for three major xanthones, HM - 1, HM - 2, and HM - 3, respectively. Conclusion: This method is simple, sensitive, reliable and reproducible. It can be applied to study the quality control of Halenia elliptica.