Objective: To establish a method of thin-layer chromatographic identification, HPLC fingerprints and a method of the content determination of 13 chemical constituents (chlorogenic acid, caffeic acid, ferulic acid, senkyunolide I, senkyunolide H, coniferyl ferulate, senkyunolide A, butylphthalide, sedanolide, Z-ligustralactone, butenylylphthalide, levistilide A, and linoleic acid) in Ligusticum sinense Oliv. cv. Chaxiong Mss. and to provide a basis for the quality control of Ligusticum sinense Oliv. cv. Chaxiong Mss. Methods: Thin-layer chromatography was used for the qualitative identification of senkyunolide I, scopoletin, ferulic acid, levistilide A and Z-ligustilide in Ligusticum sinense Oliv. cv. Chaxiong Mss. using n-hexane, ethyl acetate and acetic acid (10∶5∶0.5) as the mobile phase. The separation was carried out on an Acutfex PA-C18 column (250 mm×4.6 mm, 5 μm), with gradient elution of 0.1% aqueous phosphoric acid solution and acetonitrile at a flow rate of 1 mL·min-1. The column temperature was 30 ℃, the injection volume was 10 μL, and the detection wavelengths were 210 nm and 285 nm. The fingerprints of 54 batches of Ligusticum sinense Oliv. cv. Chaxiong Mss. were constructed. SPSS and SIMCA software were used for the chemical pattern recognition analysis, and 13 chemical components were determined at the same time. Results: A thin-layer chromatographic method was established for the identification of senkyunolide I, scopoletin, ferulic acid, levistilide A and Z-ligustilide in Ligusticum sinense Oliv. cv. Chaxiong Mss. The HPLC fingerprints of Ligusticum sinense Oliv. cv. Chaxiong Mss. were established, 21 common peaks were found, 13 common peaks were identified, and the similarities of all batches of the herbs were above 0.9, except sample S47. The herbs could be roughly divided into four groups according to the collection time and altitude by clustering analysis. OPLS-DA screened out seven differential constituents: peak 17(Z-ligustilide), peak 13 (senkyunolide A), peak 12 (coniferyl ferulate), peak 5 (ferulic acid), peak 6, peak 16 (sedanolide), and peak 2 (chlorogenic acid). A method was established for the determination of chlorogenic acid, caffeic acid, ferulic acid, senkyunolide I, senkyunolide H, coniferyl ferulate, senkyunolide A, butylphthalide, sedanolide, Z-ligustralactone, butenylylphthalide, levistilide A and linoleic acid in Ligusticum sinense Oliv. cv. Chaxiong Mss. with good linearity, precision, stability, reproducibility, and spiked recoveries. And the content ranges of the above-mentioned compounds in the herbs were 0.03-3.80 mg·g-1, 0.004-0.055 mg·g-1, 0.17-0.82 mg·g-1, 0.08-0.57 mg·g-1, 0.01-0.19 mg·g-1, 0.04-2.51 mg·g-1, 1.37-11.64 mg·g-1, 0.15-0.58 mg·g-1, 0.18-4.22 mg·g-1, 2.69-9.53 mg·g-1, 0.15-0.59 mg·g-1, 0.07-0.62 mg·g-1 and 0.31-6.04 mg·g-1, respectively. Conclusion: The method of thin-layer chromatography, HPLC fingerprints, and the determination method of the 13 constituents in Ligusticum sinense Oliv. cv. Chaxiong Mss. are simple, accurate and reliable, and can provide a basis for the evaluation of the quality of Ligusticum sinense Oliv. cv. Chaxiong Mss..
WANG Tang-xun
,
ZHANG Guan-sheng
,
YANG Jian-bo
,
CHEN Yang
,
HUANG Yu-fang
,
YANG Guang-di
,
XIA Ming-yan
,
WANG Can-jian
,
ZHANG Guo-song
. Study on the quality evaluation method of the characteristic traditional Chinese medicine Ligusticum sinense Oliv. cv. Chaxiong Mss. from Jiangxi Province*[J]. Chinese Journal of Pharmaceutical Analysis, 2024
, 44(10)
: 1665
-1678
.
DOI: 10.16155/j.0254-1793.2024-0030
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