目的 建立不同產(chǎn)地17批茺蔚子Leonuri Fructus藥材指紋圖譜,對(duì)其進(jìn)行成分研究并結(jié)合化學(xué)計(jì)量學(xué)分析進(jìn)行質(zhì)量評(píng)價(jià)。方法 通過(guò)超高效液相色譜法(UPLC),以YMC Trait C₁₈(150 mm×2.1 mm,1.9 μm)為色譜柱,乙腈-0.1%磷酸溶液為流動(dòng)相,梯度洗脫,體積流量為0.3 mL/min,柱溫為28 ℃,檢測(cè)波長(zhǎng)為205 nm,進(jìn)樣體積為2 μL。采用中藥指紋圖譜相似度評(píng)價(jià)軟件進(jìn)行相似度評(píng)價(jià),運(yùn)用化學(xué)計(jì)量學(xué)對(duì)不同產(chǎn)地茺蔚子進(jìn)行分析,同時(shí)對(duì)益母草苷B、刺桐堿、7R,8S-7′,8′-二羥基-二氫脫氫松柏醇-9-O-β-D-葡萄糖苷、落葉松脂素-9-O-β-D-葡萄糖苷、環(huán)益母草肽A進(jìn)行含量測(cè)定。結(jié)果 建立的指紋圖譜共標(biāo)識(shí)出11個(gè)共有峰,經(jīng)與對(duì)照品比對(duì),指認(rèn)6個(gè)成分;經(jīng)聚類分析和主成分分析(principal component analysis,PCA),可將不同茺蔚子聚為3類,并通過(guò)正交偏最小二乘判別法(orthogonal partial least squares-discriminant analysis,OPLS-DA)篩選出峰5、峰4、峰7(刺桐堿)、峰11(環(huán)益母草肽A)、峰10(落葉松脂素-9-O-β-D-葡萄糖苷)、峰6(益母草苷B)、峰9(7R,8S-7′,8′-二羥基-二氫脫氫松柏醇-9-O-β-D-葡萄糖苷)和峰8可以作為區(qū)分不同產(chǎn)地茺蔚子藥材的主要差異成分。17批茺蔚子中益母草苷B、刺桐堿、7R,8S-7′,8′-二羥基-二氫脫氫松柏醇-9-O-β-D-葡萄糖苷、落葉松脂素-9-O-β-D-葡萄糖苷、環(huán)益母草肽A的含量范圍分別為11.434～57.262、2.386～7.825、0.068～0.236、0.101～0.439、0.732～1.604 mg/g;經(jīng)方法學(xué)考察,各成分呈現(xiàn)良好的線性關(guān)系。結(jié)論 建立的茺蔚子指紋圖譜能反映不同產(chǎn)地的茺蔚子樣品差異,多成分含量測(cè)定方法穩(wěn)定、可靠,為茺蔚子質(zhì)量評(píng)價(jià)提供參考。

Objective To establish the fingerprint spectra of 17 batches of Leonuri Fructus (Chongweizi) from different origins. The components were studied and the quality was evaluated in combination with chemometrics analysis. Methods By ultra-performance liquid chromatography (UPLC), YMC Trait C₁₈ (150 mm × 2.1 mm, 1.9 μm) was used as the chromatographic column, and acetonitrile -0.1% phosphoric acid solution was used as the mobile phase, gradient elution was performed. The flow rate was 0.30 mL/min, the column temperature was 28 ℃, the detection wavelength was 205 nm, and the injection volume was 2 μL. Traditional Chinese medicine (TCM) fingerprint similarity evaluation software was used for similarity evaluation, and chemometrics was applied to analyze Leonuri Fructus from different origins. Meanwhile, the contents of leonuriside B, lenticin, 7R,8S-7′,8′-dihydroxydihydrodehydroconiferyl alcohol 9-O-β-D-glucopyranoside, lariciresinol-9-O-β-D-glucopyranoside, cycloleonuripeptide A were determined by similarity analysis and chemometrics analysis. Results The established fingerprint spectra identified a total of 11 common peaks. Through the identification of reference substances combined with the preparation and separation technology, a total of six components were identified by comparison with reference substances. Through cluster analysis and principal component analysis, different Leonuri Fructus can be clustered into three categories, and through OPLS-DA, peaks 5, 4, 7 (lenticin), 11 (cycloleonuripeptide A), 10 (lariciresinol-9-O-β-D-glucopyranoside), 6 (leonuriside B), 9 (7R,8S-7′,8′-dihydroxydihydrodehydroconiferyl alcohol 9-O-β-D-glucopyranoside), 8 were screened out as the main differential components for distinguishing the medicinal materials of Leonuri Fructus from different origins.The contents ranged of leonuriside B, lenticin, 7R,8S-7′,8′-dihydroxydihydrodehydroconiferyl alcohol 9-O-β-D-glucopyranoside, Lariciresinol-9-O-β-D-glucopyranoside and cycloleonuripeptide A in the 17 batches of Leonuri Fructus were 11.434—57.262, 2.386—7.825, 0.068—0.236, 0.101—0.439, 0.732—1.604 mg/g. According to the methodology, each component showed a good linear relationship. Conclusion The fingerprint spectra of Leonuri Fructus established in this paper can reflect the differences of Leonuri Fructus samples from different origins, and established multi-component content determination method is stable and reliable, which can provide a reference for the quality evaluation of Leonuri Fructus.

R286.2

2022年佛山市南海區(qū)重點(diǎn)領(lǐng)域科技攻關(guān)專項(xiàng)（南科﹝2023﹞20號(hào)-18）