高效液相色谱-二极管阵列检测器法测定食用土当归总有机酸中贝壳杉烯酸及海松酸含量

摘要

Objective To establish an HPLC-DAD method for determination of (ent)-kaur-16-en-19-oic acid and 15-dien-19-oic acid in total organic acids from the root of Aralia cordata.Methods RP-HPLC method was carried out,YMC-Pack ODS-AQ column(250 mm × 4.6 mm,5 μm)was adopted,the mobile phase was acetonitrile - 0.1％ phosphoric acid(76:24),the detection wavelength was 202 nm,the flow rate was 1.0 mL/min,the column temperature was 30 ℃,and the sample size was 15 μL.Results (Ent)-kaur-16-en-19-oic acid and 15-dien-19-oic acid had good linear relationships in the ranges of 2.257-4.514 μg(R2=0.9996),2.839-5.678 μg(R2=0.9996),respectively,the average recoveries were 100.30％ and 99.65％,and the RSDs were 1.68％ and 1.46％.The average contents of (ent)-kaur-16-en-19-oic acid and 15-dien-19-oic acid were 19.23％,27.64％ in 10 batches of total organic acids,the contents of these two components were not less than 17.00％ and 24.00％,respectively.Conclusion It is the first time to use HPLC-DAD method for determining (ent)-kaur-16-en-19-oic acid and 15-dien-19-oic acid in total organic acids from the root of Aralia cordata,this method is simple,sensitive,accurate and repeat-able,which can provide basis for establishing standard of quality control for total organic acids from the root of Aralia cordata.%目的 建立测定食用土当归总有机酸中贝壳杉烯酸及海松酸含量的高效液相色谱-二极管阵列检测器(HPLC-DAD)法.方法 采用反相高效液相色谱法,使用YMC-Pack ODS-AQ色谱柱(250 mm×4.6 mm,5μm),以乙腈-0.1％磷酸水溶液(76:24)为流动相,检测波长为202 nm,流速为1.0 mL/min,柱温为30℃,进样量为15μL.结果 贝壳杉烯酸及海松酸进样量分别在2.257～4.514μg(R2=0.9996)和2.839～5.678μg(R2=0.9996)范围内与峰面积线性关系良好,平均回收率分别为100.30％和99.65％,RSD分别为1.68％和1.46％.10批食用土当归总有机酸中贝壳杉烯酸和海松酸的平均含量分别为19.23％和27.64％,同时食用土当归总有机酸中贝壳杉烯酸含量均不低于17.00％,海松酸含量均不低于24.00％.结论 本研究中采用HPLC-DAD法首次测定了食用土当归总有机酸中贝壳杉烯酸及海松酸含量.该方法简便、灵敏、准确、重复性好,为食用土当归总有机酸质量标准的制订奠定了基础.