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中国药物评价 ›› 2022, Vol. 39 ›› Issue (4): 327-330.

• 评价技术与方法 • 上一篇    下一篇

UPLC-MS-MS法测定怀山药中去甲乌药碱的含量

    时雪峰, 王建树, 乔宇飞   

  1. 河南省焦作市疾病预防控制中心, 河南 焦作 454000
  • 收稿日期:2022-04-15 修回日期:2022-05-23 出版日期:2022-08-28 发布日期:2022-10-08

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

  1. Jiaozuo Center for Disease control and Prevention, Henan Jiaozuo 454000, China
  • Received:2022-04-15 Revised:2022-05-23 Online:2022-08-28 Published:2022-10-08

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 C18超高效液相色谱柱(150 mm×2.1 mm,1.7 μm),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=0.999 3),检出限为0.3 μg·kg-1,定量限为1 μg·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。

关键词: font-size:medium, ">去甲乌药碱;怀山药;超高效液相色谱-串联质谱(UPLC-MS-MS

Abstract: 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 C18 ultra high performance chromatographic column (150 mm×2.1 mm,1.7 μm) 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=0.999 3) in the range of 1~100 μg·L-1.The LOD for higenamine was 0.3 μg·kg-1,The LOQ for higenamine was 1.0 μg·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.

Key words: Higenamine, Huai rhizoma dioscorea, Ultra-performance liquid chromatography tandems mass spectrometry(UPLC-MS-MS)

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