道地产补骨脂-肉豆蔻药对中7个指标成分同时测定及其化学成分的初步鉴别  

Simultaneous Determination of Seven Chemical Markers and Preliminary Identification of Chemical Constituents in Daodi Psoraleae Fructus-Myristicae Semen Chinese Drug Pair

作　　者：高家荣[1] 杨晓旭[2] 吴溪[1] 魏良兵[1] 韩燕全[1] 宋俊梅[2] 

机构地区：[1]安徽中医药大学第一附属医院/国家中医药管理局中药制剂三级实验室,安徽合肥230031 [2]安徽中医药大学药学院,安徽合肥230038

出　　处：《中药材》2015年第9期1959-1963,共5页Journal of Chinese Medicinal Materials

基　　金：安徽中医药大学科学研究基金(2015fy003)

摘　　要：目的：同时测定道地产补骨脂-肉豆蔻药对中7个指标成分含量,并对其化学成分进行初步归属和鉴定。方法：高效液相色谱法测定条件：Waters Acquity UPLC BEH C18色谱柱（100 mm×2.1 mm,1.7μm）;流动相为乙腈-水,梯度洗脱;流速0.25 m L/min;进样量2μL;柱温30℃;检测波长254 nm。液质联用法测定条件：Waters HSS T3色谱柱（100 mm×2.1 mm,1.7μm）,采用电喷雾电离离子源;正离子模式检测：m/z 500--1 200,毛细管电压为3.0k V;锥孔电压为22 k V;离子源温度为110℃;脱溶剂温度为450℃;脱溶剂气体流速为800 L/h;锥孔气流量50 L/h。结果：各指标成分在选定的浓度范围内线性关系良好,加样回收率为95.07%--98.16%,RSD为1.23%~1.97%。结论：该试验为道地产补骨脂-肉豆蔻药对的质量控制和深入研究奠定了基础。Objective： To study the simultaneous determination method of daodi Psoraleae Fructus-Myristicae Semen Chinese drug pair for the seven ingredients,and Psoraleae Fructus-Myristicae Semen Chinese drug pair on the chemical composition of initial ownership and identification. Methods： UPLC BEH C18column（ 2. 1 mm × 100 mm,1. 7 μm） was used in the determination. The flow rate was kept at 0. 25 m L/min,and 2 μL of standard and sample solution were injected in each run. The mobile phase was consisted of acetonitrile and water using a gradient elution. The UPLC/Q-TOF MS condition： Waters HSS T3（ 100 mm × 2. 1 mm,1. 7 μm）; capillary voltage 3. 0 k V（ positive ion mode） and 2. 5 k V（ negative ion mode）; Mass spectrometric detection was carried out on a Waters Xevo G2 Q /TOF mass spectrometer equipped with an ESI source operating in both positive and negative ion modes. The parameters of the mass spectrometer under the ESI mode were as follows： ion source temperature 110 ℃,cone gas flow 50 L/h,desolvation gas temperature 450℃,desolvation gas flow 800 L/h. Results： The seven chemical markers in the selected linear range had good linearity. The recoveries were in the range of 95. 07% ~ 98. 16% and RSDs were between 1. 23% ~ 1. 97%. Conclusion： It is suitable for the quality control and further studies of the herb in vivo of daodi Psoraleae Fructus-Myristicae Semen Chinese drug pair.

关 键 词：道地产补骨脂-肉豆蔻药对 多指标成分 超高效液相色谱 四极杆飞行时间质谱 物质基础 

分 类 号：R284.1[医药卫生—中药学]