Key Lab of Separation Science for Analytical Chemistry, Key Lab of Natural Medicine, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Liaoning Province. Dalian, 116023, China.
Analyst. 2012 Mar 21;137(6):1451-7. doi: 10.1039/c2an15824h. Epub 2012 Feb 2.
A non-aqueous solid phase extraction (SPE) method utilizing silica based strong cation exchange (SCX) was developed and optimized for the enrichment of alkaloids. In this method, silica based SCX SPE columns were used for the elimination of non-alkaloid compounds and the preconcentration of alkaloids from the extracts. Mass spectrometry was employed to analyze the alkaloid-enriched fraction, and results showed that the SPE method developed in this study was effective for the removal of non-alkaloids. Then, this pretreatment method was combined with high performance liquid chromatography for the quantification of scopolamine and hyoscyamine from Scopolia tangutica Maxim. The recoveries of scopolamine and (-)-hyoscyamine were 98.51% and 91.12%, respectively. Relative standard deviation values were 1.4% for scopolamine and 1.6% for (-)-hyoscyamine. The linearity was good in the 0.01-0.8 mg mL(-1) range for hyoscyamine and 0.01-0.4 mg mL(-1) range for scopolamine.
建立并优化了一种基于硅胶的强阳离子交换固相萃取(SCX)非水相固相萃取(SPE)方法,用于生物碱的富集。在该方法中,硅胶基 SCX SPE 柱用于消除非生物碱化合物并从提取物中预浓缩生物碱。采用质谱法分析生物碱富集部分,结果表明,本研究开发的 SPE 方法可有效去除非生物碱。然后,将该预处理方法与高效液相色谱法结合,用于从 Tangut 莨菪中定量检测莨菪碱和(-)-东莨菪碱。莨菪碱和(-)-东莨菪碱的回收率分别为 98.51%和 91.12%。莨菪碱和(-)-东莨菪碱的相对标准偏差值分别为 1.4%和 1.6%。莨菪碱在 0.01-0.8 mg mL(-1)范围内,东莨菪碱在 0.01-0.4 mg mL(-1)范围内具有良好的线性。