壮药一匹绸薄层鉴别和咖啡酸提取工艺及含量测定

TLC Identifi cation and Caffeic Acid Extraction Technology and Content Determination of Argyreia Aceta

目的通过用咖啡酸作为指标性的成分,建立壮药一匹绸的含量测定和薄层鉴别方法,比较壮药一匹绸在不同产地咖啡酸的含量。方法应用硅胶GF254来作为薄层鉴别的薄层板,展开剂为体积比甲苯:甲酸:乙酸乙酯(5:1.2:3)的溶剂,以365 nm紫外灯下作为观察环境。流动相:甲醇-0.1%磷酸(23:77),检测波长320 nm,含量用色谱柱Thermo SCIENTIFIC Hypersil碳十八柱(4.60×250 mm,5μm)与色谱柱Thermo SCIENTIFIC Hypersil GOLD-C18柱(4.60×250 mm,5μm)测定,柱温30℃,进样量10μL,流速1.0 mL/min。结果薄层色谱中能够验出咖啡酸,其专属性强,斑点显示清楚。咖啡酸进样量在0.015 1～0.453μg(R2=0.999 9)范围之内时,与峰面积呈现比较良好的线性关系。壮药一匹绸加样平均回收率分别为99.94%(RSD=2.68%)、97.56%(RSD=1.57%)、99.79%(RSD=2.05%)。结论此方法可以有效鉴别一匹绸,可将一匹绸中的咖啡酸准确测定。此方法具有准确度高、精密度高、显色稳定性好、重现性好、分析速度快等优点。

Objective By using caffeic acid as an indicator, the content determination and TLC identification method of Zhuang medicine silk fabric were established, and the content of caff eic acid in diff erent producing areas was compared. Methods Silica gel GF254 was used as thin layer plate for TLC identification. The expansion agent was the volume ratio of toluene to toluene: formic acid: ethyl acetate(5:1.2:3), and under the 365 nm ultraviolet lamp as the observation environment. Mobile phase: methanol-0.1% phosphoric acid(23:77), the detection wavelength is 320 nm, the content is determined by the chromatographic column Thermo SCIENTIFIC Hypersil carbon eighteen column(4.60×250 mm, 5 μm) and the Thermo SCIENTIFIC Hypersil GOLD-C18 column(4.60×250 mm, 5 μm), the column temperature is 30, and the sample volume is 10 μL. Results Caff eic acid can be detected in TLC with strong specificity and clear spots. When caff eic acid injection volume was in the range of 0.015 1 μg ~ 0.453 μg(R^2 = 0.999 9), it showed a good linear relationship with the peak area. The average recoveries of Zhuang medicine and one silk were 99.94%(RSD = 2.68%), 97.56%(RSD =1.57%) and 99.79%(RSD = 2.05%) respectively. Conclusion This method can identify a piece of silk eff ectively and accurately measure caff eic acid in a piece of silk. High accuracy, high precision, good color stability, good reproducibility, fast analysis speed and other advantages.