UPLC-MS-MS法测定怀山药中去甲乌药碱的含量  

Determination of Higenaminein in Huai Rhizoma Dioscorea by UPLC-MS-MS

作　　者：时雪峰[1] 王建树[1] 乔宇飞 SHI Xue-feng;WANG Jian-shu;QIAO Yu-fei(Jiaozuo Center for Disease control and Prevention,Henan Jiaozuo 454000,China)

机构地区：[1]河南省焦作市疾病预防控制中心,河南焦作454000

出　　处：《中国药物评价》2022年第4期327-330,共4页Chinese Journal of Drug Evaluation

摘　　要：目的:建立超高效液相色谱-串联质谱(UPLC-MS-MS)法测定怀山药中去甲乌药碱含量的测定方法。方法:样品用0.1%高氯酸溶液提取、MCX固相萃取柱净化,5%氨水甲醇溶液洗脱,洗脱液水浴上氮吹干后用50%甲醇水溶液(含0.1%甲液)复溶。采用Waters BEH C_(18)超高效液相色谱柱(150 mm×2.1 mm,1.7μm),流动相为乙腈-0.1%的甲酸水溶液进行梯度洗脱分离,柱温30℃,流速为0.3 mL·min^(-1),以非诺特罗作为内标进行定量。结果:去甲乌药碱的线性范围为1~100 ng·mL^(-1)(r=0.9993),检出限为0.3μg·kg^(-1),定量限为1μg·kg^(-1);样品加标回收率为86.8%~91.8%,相对标准偏差为2.1%。结论:本方法净化效果好,灵敏度高,线性范围广,重复性好,能够满足怀山药中去甲乌药碱含量测定要求。Objective:A method for determination of higenamine in Huai rhizoma dioscorea by ultra-performance liquid chromatography tandems mass spectrometry(UPLC-MS-MS)was established.Methods:Samples were extracted with 0.1%perchloric acid solution、purified by MCX SPE column and eluted with 5%ammonia methanol solution.After the eluent was blown dry with nitrogen in the water bath,it was redissolved with 50%methaool aqueous solution(containing 0.1%formic acid).Waters BEH C_(18)ultra high performance chromatographic column(150 mm×2.1 mm,1.7μm)was used for seperation.The mobile phase was acetonitrile-0.1%formic acid aqueous solution by gradient elution with the column temperature of 30℃and the flow rate of 0.3 mL·min^(-1).Fenoterol was used as the internal standard for quantification.Results:Higenamine showed a good linearity(r=0.9993)in the range of 1~100μg·L^(-1).The LOD for higenamine was 0.3μg·kg^(-1),The LOQ for higenamine was 1.0μg·kg^(-1).The recovery ranged from 86.7%~92.3%and RSD ranged from 2.1%to 4.2%.Conclusion:This method is suitable for determination of higenamine in Huai rhizoma dioscorea.

关 键 词：去甲乌药碱 怀山药 超高效液相色谱-串联质谱(UPLC-MS-MS) 

分 类 号：R284.2[医药卫生—中药学] R927.2[医药卫生—中医学]