色谱

色谱 ›› 2011, Vol. 29 ›› Issue (02): 176-179.DOI: 10.3724/SP.J.1123.2011.00176

• 技术与应用 • 上一篇    下一篇

高效液相色谱-串联质谱法同时测定夏天无中的4种生物碱

沈燕1*, 韩超2, 刘翠平2, 周永芳2, 夏碧琪2, 朱振瓯2, 刘爱丽1   

  1. 1. 温州大学化学与材料工程学院, 浙江 温州 325035; 2. 温州出入境检验检疫局, 浙江 温州 325027
  • 收稿日期:2010-10-11 修回日期:2010-11-22 出版日期:2011-02-28 发布日期:2007-03-25
  • 通讯作者: 沈燕,硕士,讲师,主要从事色谱分析方面的研究.
  • 基金资助:

    温州市科技局科研项目

Simultaneous determination of four alkaloids in Corydalis decumbens (Thunb.) Pers. by high performance liquid chromatography-tandem mass spectrometry

SHEN Yan1*, HAN Chao2, LIU Cuiping2, ZHOU Yongfang2, XIA Biqi2, ZHU Zhenou2, LIU Aili1   

  1. 1. College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou 325035, China; 2. Wenzhou Entry-Exit Inspection and Quarantine Bureau, Wenzhou 325027, China
  • Received:2010-10-11 Revised:2010-11-22 Online:2011-02-28 Published:2007-03-25

PDF

541

被引次数

12

摘要： 建立了高效液相色谱-电喷雾串联四极杆质谱同时测定夏天无中4种生物碱的分析方法。夏天无样品用甲醇超声提取,提取溶液过滤并用甲醇稀释后分析。色谱分离采用C18反相色谱柱(150 mm×2.1 mm, 3.5 μm),流动相为0.2%乙酸水溶液和乙腈,梯度洗脱。电喷雾串联质谱在多反应监测(MRM)模式下检测目标分析物,以保留时间和特征离子对(母离子和两个碎片离子)信息比较进行定性分析和定量分析。4种生物碱的检出限(LOD)为0.02～0.2 μg/L,定量限(LOQ)为0.07～0.66 μg/L,加标回收率为93.6%～103.5%,相对标准偏差小于3.8%。该方法简便、准确、灵敏,可用于夏天无中药材的质量控制。

关键词: 高效液相色谱-电喷雾串联质谱, 生物碱, 夏天无；中药材

Abstract: A method for the analysis of 4 alkaloids in Corydalis decumbens (Thunb.) Pers. was developed by high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-MS/MS). The sample was extracted in methanol by ultrasonic, filtered and diluted with methanol for further analysis. The analysis was performed on a C18 column (150 mm×2.1 mm, 3.5 μm) using a gradient elution program with the mobile phase of 0.2% acetic acid solution and acetonitrile. The analyte was determined by an electrospray ionization tandem mass spectrometry in multiple reactions monitoring (MRM) mode. The qualitative and quantitative analyses were based on the retention times and characteristic ion pairs consisting of one parent ion and two fragment ions of the analyte. The limits of detection (LODs) for 4 alkaloids were in the range of 0.02~0.2 μg/L, and the limits of quantification (LOQs) were in the range of 0.07~0.66 μg/L. The average recoveries were in the range of 93.6%～103.5% for 4 alkaloids with the relative standard deviations below 3.8%. This method is reliable, sensitive and reproducible, and it can be used for the quality control of Corydalis decumbens (Thunb.) Pers. sample.

Key words: Corydalis decumbens (Thunb.) Pers., LC-MS/MS, Alkaloids