GC/MS法测定草豆蔻中桤木酮的含量  

Determination of the content of Alnusone in Alpinia katsumadai Hayata by GC/MS

作　　者：王睿 张雨佳 冯雪松[1] WANG Rui;ZHANG Yu-jia;FENG Xue-song(School of Pharmacy,China Medical University,Shenyang,Liaoning 110122,China)

机构地区：[1]中国医科大学药学院,辽宁沈阳110122

出　　处：《时珍国医国药》2018年第11期2594-2597,共4页Lishizhen Medicine and Materia Medica Research

基　　金：辽宁省自然科学基金(20170541027);中华医学会医学教育分会和中国高等教育学会医学教育专业委员会医学教育研究重点课题(2016A-YX004);辽宁省社会科学规划基金项目(L17BGL034);辽宁省普通高等学校本科教学改革研究项目(2016-346)

摘　　要：目的对中药材草豆蔻中桤木酮进行鉴别及含量测定。方法采用GC/MS法测定草豆蔻中桤木酮的含量。色谱柱为SH-Rxi-5Sil MS色谱柱(30m×0.25mm×0.25μm,日本岛津公司);载气为氦气,总流速为20ml/min;柱温采取程序升温:起始温度100℃,保持3min,以30℃/min升至260℃,保持6min,再以10℃/min升至280℃,保持6min;进样口温度为250℃;接口温度270℃;电子轰击(EI)离子源;离子源温度200℃;数据采集方式SIM模式。结果该方法中桤木酮在2.463~98.50μg/ml与峰面积线性关系良好(r=0.9941);定量限(S/N=10)为0.657μg/ml,检测限(S/N=3)为0.164μg/ml;精密度、稳定性、重复性试验的RSD在0.5623%~3.4259%之间;平均回收率(n=6,RSD=1.4%)为93.16%。结论该方法灵敏度高、专属性强、重现性好及检测成本低,可用于草豆蔻中桤木酮的鉴别及含量测定。Objective To develop a sensitive gas chromatography tandem mass spectrometry(GC-MS)method for the determination of Alnusone in Alpinia katsumadai Hayata.Methods Alnusone were extracted from samples by methyl alcohol after Ultrasonic extraction,with caffeine serving as an internal standard.The analytes went through the column of SH-Rxi-5 Sil MS(30 m×0.25 mm×0.25μm,Shimadzu)using helium as carrier gas and were analyzed under the selected ion monitoring mode using the electrospray ionization(ESI)technique.The column temperature was initially maintained at 100℃for 3 min,then increased to260℃at the rate of 30℃per min and maintained for 6 min,finally increased to 280℃at the rate of 10℃per min and maintained for 6 min.Injector temperature was set at 250℃and interface at 270℃respectively.Results The linear range of Alnusone was 2.463~98.50μg/ml(r=0.9941).The LOD was 0.164 ng and the LOQ was 0.657 ng.Conclusion The results indicated that the method were specific,accurate and reproducible for the determination of Alnusone.

关 键 词：草豆蔻 桤木酮 气质联用 含量测定 

分 类 号：R284.1[医药卫生—中药学]