[關(guān)鍵詞]
[摘要]
目的 建立黑龍骨Periploca forrestii莖葉(PFSL)中7個成分的UPLC測定方法 ,并對結(jié)果進(jìn)行化學(xué)計量學(xué)分析。方法采用Agilent Eclipse Plus C18色譜柱(100 mm×2.1 mm,1.8 mm),以0.1%磷酸水-乙腈為流動相梯度洗脫,體積流量0.2 mL·min−1,進(jìn)樣量0.8 mL,柱溫30℃;采用切換波長法測定15批PFSL中新綠原酸、綠原酸、咖啡酸、隱綠原酸、異槲皮苷、紫云英苷及異綠原酸C的含量,結(jié)合聚類分析(HCA)、主成分分析(PCA)和正交偏最小二乘法-判別分析(OPLS-DA)對含量測定結(jié)果進(jìn)行綜合評價。結(jié)果 新綠原酸、綠原酸、咖啡酸、隱綠原酸、異槲皮苷、紫云英苷及異綠原酸C在0.030 40~1.216 00、0.012 60~1.008 00、0.001 24~0.024 80、0.015 20~0.496 00、0.011 20~0.179 20、0.007 84~0.117 60、0.003 64~0.136 00 mg·mL−1線性關(guān)系良好(R2>0.999 0),平均加樣回收率分別為96.01%、98.93%、98.52%、98.94%、98.06%、96.22%、98.20%,RSD分別為2.29%、3.13%、3.22%、2.71%、1.92%、2.86%、2.38%;質(zhì)量分?jǐn)?shù)分別為1.413 1~12.257 1、0.912 1~10.090 6、0.042 4~0.314 8、0.926 6~8.537 9、0.350 6~3.337 0、0.176 4~0.610 0、0.253 1~1.257 6 mg·g−1?;瘜W(xué)計量學(xué)分析結(jié)果顯示,15批PFSL樣品聚為3類,隱綠原酸、咖啡酸、紫云英苷、新綠原酸、綠原酸、異槲皮苷為15批樣品中的主要差異成分。結(jié)論 建立的UPLC含量測定方法穩(wěn)定,結(jié)合化學(xué)計量學(xué)方法可為PFSL質(zhì)量評價提供參考。
[Key word]
[Abstract]
Objective To establish an UPLC content determination method of seven components in Periploca forrestii stem-leaf (PFSL), and analyze the content determination results by chemometrics method. Methods The analysis was carried out on Agilent Eclipse Plus C18 column (100 mm×2.1 mm, 1.8 mm). The mobile phase was 0.1% phosphoric acid- acetonitrile with gradient elution. The volume flow was 0.2 mL·min−1, the injection volume was 0.8 μL, and the column temperature was 30℃. Measuring the content of neochlorogenic acid, chlorogenic acid, caffeic acid, cryptochlorogenic acid, isoquercitrin, astragalin and isochlorogenic acid C in 15 batches of PFSL by wavelength switching method. The content determination results were comprehensively analyzed using hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA).ResultsNeochlorogenic acid, chlorogenic acid, caffeic acid, cryptochlorogenic acid, isoquercitrin, astragalin and isochlorogenic acid C showed good linear relationship (R2>0.999 0) within the ranges of 0.030 40—1.216 00, 0.012 60—1.008 00, 0.001 24—0.024 80, 0.015 20—0.496 00, 0.011 20—0.179 20, 0.007 84—0.117 60, 0.003 64—0.136 00 mg·mL−1, whose average recoveries were 96.01%, 98.93%, 98.52%, 98.94%, 98.06%, 96.22% and 98.20%, with RSD values of 2.29%, 3.13%, 3.22%, 2.71%, 1.92%, 2.86%, 2.38%, respectively. Their mass fractions were 1.413 1—12.257 1, 0.912 1—10.090 6, 0.042 4—0.314 8, 0.926 6—8.537 9, 0.350 6—3.337 0, 0.176 4—0.610 0 and 0.253 1—1.257 6 mg·g−1. The chemometrics analysis results showed that 15 batches of PFSL could be clustered into three categories, cryptochlorogenic acid, caffeic acid, astragalin, neochlorogenic acid, chlorogenic acid and isoquercitrin were the main differential components in 15 batches of samples. Conclusion The established method for the determination of multi-component content in PFSL is stable, which can provide reference for the quality evaluation of PFSL combined with chemometrics method.
[中圖分類號]
R284.1
[基金項目]
貴州省科技計劃項目[黔科合基礎(chǔ)-ZK(2022)一般475號];貴州省教育廳滾動支持省屬高??蒲衅脚_團(tuán)隊項目[黔教技(2022)024號]