HPLC法测定硫磺熏蒸与未熏蒸北沙参中5种香豆素类成分的含量

Contents Determination of 5 Coumarins in Sulphur-fumigated and No Sulphur-fumigated Glehnia littoralis by HPLC

目的:建立测定硫磺熏蒸与未熏蒸北沙参中5种香豆素类成分含量的方法,考察硫磺熏蒸对北沙参中香豆素类成分的影响。方法:采用高效液相色谱法。色谱柱为Hypersil ODS C18,流动相为乙腈-0.1%磷酸(梯度洗脱),流速为1.0 ml/min,检测波长为295 nm,柱温为30℃,进样量为20μl。结果:补骨脂素、花椒毒素、佛手柑内酯、欧前胡素、异欧前胡素的质量浓度分别在0.121 5~12.15、0.389~38.9、0.055~5.5、0.070 5~7.05、0.092 5~9.25μg/L范围内与各自峰面积呈良好的线性关系(r≥0.999 7);精密度试验的RSD<1.0%,重复性、稳定性试验的RSD<3.0%;加样回收率为98.01%~101.97%,RSD<3.0%(n=6)。结论:硫磺熏蒸后北沙参中香豆素类成分含量明显减少。该方法简单、准确,可用于硫磺熏蒸与未熏蒸北沙参的质量控制。

OBJECTIVE： To establish a method for the contents determination of 5 coumarins in sulphur-fumigated and no sul- phur-fumigated Glehnia littoralis, and investigate the effect of sulphur fumigation on the coumarins in G. littoralis. METHODS： HPLC was performed on the column of Hypersil ODS C^8 with mobile phase of acetonitrile-0.1% phosphoric acid （gradient elu- tion） at a flow rate of 1.0 ml/min, detection wavelength was 295 nm, column temperature was 30 ~C, and the volume was 20 μl. RESULTS： The linear range was 0.121 5-12.15 pg/L for psoralen, 0.389-38.9 μg/L for xanthotoxin, 0.055-5.5 μg/L for bergapten, 0.070 5-7.05μg/L for imperatorin and 0.092 5-9.25 μg/L for isoimperatorin（r≥0.999 7）; RSD of precision test was lower than 1.0, RSDs of reproducibility and stability tests were lower than 3.0; recovery was 98.01%-101.97% （RSD〈3.0% ,n-6）. CON- CLUSIONS：The content of coumarins in G. littoralis was obviously decreased after sulphur fumigation, the method is simple and accurate, and canbe used for the quality control of sulphur-fumigated and no sulphur-fumigated G. littoralis.