红外辅助提取-HPLC法测定卷柏中穗花杉双黄酮的含量

Determination of content of amentoflavone in Selaginella tamariscina by infrared-assisted extraction method coupled with HPLC

目的建立红外辅助提取-高效液相色谱(IRAE-HPLC)法,用于提取并测定卷柏药材中穗花杉双黄酮的含量。方法将卷柏药材粉碎过筛,取0. 25 g卷柏粉末,用40 m L体积分数为80%的乙醇进行提取,提取时间25 min,红外灯功率为250 W。将提取液通过高效液相色谱仪进行分离分析,色谱柱为XtimateTMC18色谱柱,流动相:甲醇-0. 1%H_3PO_4(60∶40),流速1 mL·min^(-1),检测波长330 nm。结果穗花杉双黄酮在0. 005~0. 045 g·L^(-1)内线性关系良好(r=0. 999 8),定量限为0. 005 g·L^(-1)。用该方法测得卷柏中穗花杉双黄酮含量为0. 29%(RSD=2. 07%),平均加样回收率为101. 67%(RSD=2. 63%)。结论本实验建立的IRAE-HPLC法的提取效率较高,分析方法可靠,适宜推广应用。

AIM To develop an infrarced-assisted extraction method coupled with HPLC（IRAE-HPLC） for the extraction and determination of amentoflavone in Selaginella tamariscina. METHODS The medicinal materials of amentoflavone were smashed and sifted. The 0.25 g powder of amentoflavone was extracted by IRAE with 40 mL 80% C2H5OH, using extraction condition of 250 W and 25 min. The extraction was determined by HPLC on a XtimateTM C18 column with methanol- 0. 1% phosphoric acid aqueous（60： 40） as the mobile phase. Detection wavelength was 330 nm. The flow rate was 1mL·min^-1 RESULTS The standard curve for amentoflavone was linear over the range of 0.005-0.045 g·L^-1（r=0.999 8） and LOQ was0.005g·L^-1. The content ofament-oflavone was 0.29% , with RSD = 2.07%. The recovery of amentoflavone was 101.67% , with RSD = 2.63%. CONCLUSION The method has higher extraction efficiency and the analytical method is reliable. The IRAE-HPLC is suitable for popularization and application. [ KEY WORDS] infrarced-assisted extraction; amentoflavone ; Selaginella tamariseina