HPLC法同时测定不同产地佛手中5个成分的含量  

Simultaneous determination of 5 components in Fructus Citris Sarcodactylis from different habitats by HPLC

作　　者：魏莹[1] 陈珍[1] 杨兰[1] 杨春艳 刘福[2] 张帆[1] 

机构地区：[1]川北医学院药学院药物研究所,南充637000 [2]川北医学院附属医院药剂科,南充637000

出　　处：《药物分析杂志》2017年第12期2180-2184,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：川北医学院2015年校级科研发展项目(CBY15-A-YB22);川北医学院博士项目(201402)

摘　　要：目的:建立HPLC波长切换法同时测定佛手药材中柚皮苷、橙皮苷、6,7-二甲氧基香豆素、5,7-二甲氧基香豆素和佛手柑内酯的含量。方法:采用Diamonsil C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为乙腈(A)-0.1%醋酸水(B),二元梯度洗脱(0~15 min,18%A→26%A;15~18 min,26%A→49%A;18~25 min,49%A;25~28 min,49%A→100%A),流速1.0 m L·min-1,柱温30℃,波长切换(0~15 min,在283 nm波长下检测柚皮苷和橙皮苷;15~28 min,在320 nm波长下检测6,7-二甲氧基香豆素、5,7-二甲氧基香豆素和佛手柑内酯)。结果:柚皮苷、橙皮苷、6,7-二甲氧基香豆素、5,7-二甲氧基香豆素和佛手柑内酯的进样量分别在9.3~186.6μg(r=0.999 8)、40.6~812.8μg(r=0.999 8)、8.4~167.7μg(r=0.999 9)、80.6~1 612.8μg(r=0.999 9)和4.3~86.4μg(r=0.999 9)范围内呈良好的线性关系;平均回收率(n=6)分别为95.5%、98.9%、95.8%、100.2%、97.7%,RSD分别为3.0%、2.6%、1.8%、2.6%、3.0%。11批佛手样品中柚皮苷、橙皮苷、6,7-二甲氧基香豆素、5,7-二甲氧基香豆素和佛手柑内酯含量测定结果分别为0.019%~0.068%、0.028%~0.275%、0~0.075%、0.094%~0.501%、0.002~0.034%。结论:本法可用于佛手药材中柚皮苷、橙皮苷、6,7-二甲氧基香豆素、5,7-二甲氧基香豆素和佛手柑内酯的含量测定。Objective： To develop a method for simultaneous determination of naringin, hesperidin, 6, 7-dimethoxyeoumarin, 5,7-dimethoxycoumarin and bergapten in Fructus Citris Sarcodactylis by HPLC with wavelength switching. Methods： The separation was performed on a Diamonsil C18 column （ 250 mm ×4.6 mm,5μm ） and the column temperature was set at 30℃. The mobile phase was composed of acetonitrile and 0.1% acetic acid with gradient elution at a flow rate of 1.0 mL·min-1. The detection wavelength was set at 283 nm （ 0-15 min ）for naringin and hesperidin, then at 320 nm （ 15-28 min ）for 6, 7-dimethoxycoumarin, 5,7-dimethoxycoumarin and bergapten. Results： Naringin, hesperidin, 6, 7-dimethoxycoumarin, 5,7-dimethoxycoumarin and bergapten had good linear relationship in the ranges of 9.3-186.6 μg（ r=0.999 8 ）, 40.6-812.8 μg（ r=0.999 8 ）, 8.4-167.7μg（ r=0.999 9 ）, 80.6-1 612.8μg（ r=0.999 9 ）and 4,3-86.4μg（ r=0.999 9 ）, respectively. And the average recoveries （ n=6 ） of the five components were 95.5% with RSD of 3.0%, 98.9% with RSD of 2.6%, 95.8% with RSD of 1.8%, 100.2% with RSD of 2.6% and 97.7% with RSD of 3.0%, respectively. The contents in 11 Fructus Citris Sareodactylis samples were 0.019%-0.068% for naringin, 0.028%-0.275% for hesperidin, 0-0.075%% for 6, 7-dimethoxycoumarin, 0.094%-0.501% for 5,7-dimethoxycoumarin and 0.002%-0.034% for aurapten. Conclusion： The method could be applied to the determination of naringin, hesperidin, 6,7-dimethoxycoumarin, 5, 7-dimethoxycoumarin and bergapten in Fructus Citris Sarcodactylis.

关 键 词：佛手 柚皮苷 橙皮苷 二甲氧基香豆素 佛手柑内酯 方法学验证 中药材多成分测定 高效液相色谱法 波长切换法 

分 类 号：R917[医药卫生—药物分析学]