加速溶剂萃取/气相色谱-三重四极杆质谱测定石菖蒲中的α-细辛脑和β-细辛脑  

Applicability of accelerated solvent extraction for analysis of α-asarone and β-asaronein Acorus tatarinowii Schott with gas chromatography-triple quadrupole mass spectrometry

作　　者：廖且根[1] 李伟红[1] 孙吉昌 罗林广[1] 

机构地区：[1]江西省农业科学院农产品质量安全与标准研究所,南昌330200 [2]江西省疾病控制中心,南昌330029

出　　处：《药物分析杂志》2013年第7期1231-1234,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：江西省农业科学院创新基金(2010CJJ012)

摘　　要：目的:建立加速溶剂萃取/气相色谱-三重四极杆质谱(GC-MS/MS)测定石菖蒲中的细辛脑含量方法。方法:为了取得最佳的萃取效果,优化萃取溶剂、温度、静态萃取时间和次数等加速溶剂萃取条件。萃取液稀释后直接通过GC-MS/MS分析,多反应监测模式检测细辛脑,以保留时间和特征离子对(母离子(m/z)为208.2和2个子离子(m/z)为192.8和164.8)信息比较进行定性定量分析,外标法定量。结果:选择甲醇为萃取试剂,120℃静态萃取5.0 min共2次,则萃取效率最佳。细辛脑在DB-1701毛细管柱上实现基线分离,α-细辛脑和β-细辛脑检测限依次为0.2μg·L-1和0.5μg·L-1。结论:本法提取效率高,定量准确,定性可靠,可用于石菖蒲中细辛脑的含量测定及质量评价。Objective： To develop a sensitive and reliable method for the analysis of asarone in Acorus tatarinowii Schott using accelerated solvent extraction（ASE） and gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS）.Methods： The ASE parameters（extraction solvent and temperature,static time and cycle） were optimized in order to maximize the extraction efficiency.The ASE extract was diluted with methanol.The asarone was determined by GC-MS / MS in multiple reactions monitoring（MRM） modes.The qualitative and quantitative analysis was performed base on the retention time and the characteristic ion-pairs consisting of one precursor ion（m/z） of 208.2 and two product ions（m/z） of 192.8 and 164.8.The contents of asarone were quantified by external standard method.Results： Optimal results were achieved by using methanol as extraction solvent at a temperature of 120 ℃,and applying two cycle of extraction with a static time of 5.0 min.A good GC separation was achieved using a DB-1701 capillary column.The detection limits of α-asarone and β-asarone were 0.2 μg·L-1 and 0.5 μg·L-1,respectively.Conclusion： The method is highly efficient in extraction,accurate quantitative and reliable qualitative,which can be used for determination of asarone in Acorus tatarinowii Schott.

关 键 词：气相色谱-三重四极杆质谱 加速溶剂萃取 石菖蒲 细辛脑 

分 类 号：R917[医药卫生—药物分析学]