| Structure Identification: |
| Zhongguo Zhong Yao Za Zhi. 2014 May;39(9):1650-5. | | [Quantitative determination of 5 active ingredients in different harvest periods of Ligusticum chuanxiong by HPLC].[Pubmed: 25095378] | A simple and quick method is described for the determination of ferulic acid, senkyunolide I, senkyunolide H, Senkyunolide A and ligustilide in rhizomes of Ligusticum chuanxiong.
METHODS AND RESULTS:
The 5 active ingredients in the sample was extracted using 40% ethanol and analyzed by reversed-phase high performance liquid chromatography (HPLC). Chromatography separation was performed using Agilent 1100 series HPLC system with a Symmetry C18 column and gradient elution with a mixture of three solvents : solvent A, acetonitrile, solvent B, methanol and solvent C, 1% aqueous acetic acid, 0 min to 5 min A: B: C 20: 40: 40, 5 min to 30 min A: B: C 60 to 100 : 0 : 40 to 0. The effluent was monitored using a VWD detector set at 321 nm (0-4.3 min) and 275 nm (4.31-30 min). The flow rate was set at 1 mL x min(-1) and the injection volume was 10 microL. The column temperature was maintained at 35 degrees C. The calibration curve was linear (r > or = 0.99) over the tested ranges. The average recovery was 94.44%-103.1% (n = 6). The method has been successfully applied to the analysis in different harvest periods of L. chuanxiong samples.
CONCLUSIONS:
In this paper, single-factor randomized block design to study the 5 components content of L. chuanxiong on ten collecting stages. For the L. chuanxiong collected from April 15th to May 30rd, the content of 5 ingredients increased primarily, and then decreased. Determine the appropriate harvest time has important significance to the promotion of the quality of L. chuanxiong. | | Chem Pharm Bull (Tokyo). 2005 Nov;53(11):1480-3. | | Identification and comparative determination of senkyunolide A in traditional Chinese medicinal plants Ligusticum chuanxiong and Angelica sinensis by HPLC coupled with DAD and ESI-MS.[Pubmed: 16272738] |
METHODS AND RESULTS:
Using the HPLC/DAD/ESI/MS method, the qualitative and quantitative analysis of Senkyunolide A (SA) in the rhizomes of Ligusticum chuanxiong (Rhizoma chuanxiong; CX) and roots of Angelica sinensis (DG) was established. As a result, it was found that Senkyunolide A is a characteristic standard compound for the quality evaluation and chemical differentiation between CX and DG. Methanol was chosen in the preparation of standard solutions and extraction of samples based on the stability data. The identity of Senkyunolide A in CX and DG was unambiguously determined based on the quasimolecular ions in ESI-MS. A comprehensive validation of the method, including sensitivity, linearity, reproducibility and recovery, was conducted using the optimized chromatographic conditions. The linear calibration curve was acquired with R2>0.999 and limit of detection (S/N=3) was estimated to be 12.5 mug/g. The reproducibility was evaluated by repeated sample injection and replicated analysis of samples with the relative standard deviation (RSD) value found within 0.68%. The recovery rates of Senkyunolide A varied within the range of 96.91-101.50% with RSD less than 2.38%. In the present work, the contents of Senkyunolide A were quantified within 3.94-9.14 mg/g and 0.108-0.588 mg/g for 12 batches each of CX and DG.
CONCLUSIONS:
The results demonstrated that Senkyunolide A is a useful standard compound for the quality evaluation and chemical differentiation between CX and DG. The analytical procedure is precise and reproducible and thus suitable for the analysis of a large number of samples. |
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