1.Isolation and Identification the Compositions of Alkaloids in Acorus tatarinowii
Xiaoling HU ; Yi TANG ; Jinbin YUAN
China Pharmacy 2019;30(5):642-645
OBJECTIVE: To isolate and identify the compositions of alkaloids in Acorus tatarinowii, and to lay the foundation for further study of its pharmacological activity. METHODS: The compositions of alkaloids from A. tatarinowii was separated by cation exchange resin. UPLC-MS method was used to identify the alkaloids. The separation was performed on a Agilent Zorbax Eclipse Plus-C18 column with mobile phase consisted of 0.1% formic acid-acetonitrile (gradient elution) at a flow rate of 0.3 mL/min. The column temperature was 30 ℃, and the injection volume was 1 μL. ESI ion source was used to detect the fragments, the ion mode scan was positive. Peakview 1.2 and other softwares were used to analyze the compositions of alkaloids. RESULTS: 86 compositions were separated and 5 alkaloids were identified, such as tatarine A, N-trans-feruloyltyramine, N-lauryldiethanolamine, phytosphingosine and 5-butyluridine. CONCLUSIONS: The results of the study lay a foundation for the study of pharmacological activity of alkaloids from A. tatarinowii.
2.Content determination of 3 alkaloids in different origins of Tibetan Corydalis pallida by UPLC-MS/MS
Huan HUANG ; Xuhang YI ; Yi QIU ; Yongchang XIONG ; Huijuan WANG ; Zhinan CAI ; Zhuoma DAWA ; Jinbin YUAN
China Pharmacy 2023;34(7):832-836
OBJECTIVE To establish and apply a method for simultaneous determination of the contents of dicentrine, protopine and coptisine in Tibetan Corydalis pallida of different origins, and to provide reference for origin determination and quality control of the kind of medicinal materials. METHODS Ultra performance liquid chromatography-tandem quadrupole mass spectrometry method was used. The determination was performed on Agilent EC-C18 column (100 mm×2.1 mm, 2.7 μm) with mobile phase consisted of acetonitrile-0.1% formic acid by gradient elution. The flow rate was 0.2 mL/min, and the column temperature was set at 35 ℃ . MS detection was carried out by electrospray ionization in positive modes, multiple reaction monitoring mode was used for quantitative analysis. RESULTS The injection mass concentrations of dicentrine, protopine, coptisine ranged from 5.88 to 117.60, 53.70 to 1 074.00, and 4.85 to 97.00 ng/mL, respectively, showing a good linear relationship with their respective peak areas (r=0.998 2, 0.991 9, and 0.999 6, respectively). The limits of quantitation were 2.35, 1.07 and 1.46 ng/mL; the limits of detection were 1.17, 0.54, 0.49 ng/mL, respectively. RSDs of precision, stability (24 h) and repeatability tests were all lower than 2.0%. The average recovery rates were 97.41%, 98.89% and 105.44%( all RSDs<5.0%, n=6). CONCLUSIONS The established method has good selectivity and high accuracy, and is suitable for the rapid analysis of dicentrine, protopine and coptisine in Corydalis. The total contents of three alkaloids in different original medicinal materials are from high to low in order of C. chrysosphaera, C. mucronifera, C. pygmaea, C. hendersonii and C. conspersa. The alkaloid contents in C. chrysosphaera and C. mucronifera are relatively similar, but no dicentrine has been detected in C. conspersa and C. hendersonii.