HPLC法同时测定不同采集地衢枳壳中12种黄酮类成分的含量  

Simultaneous Determination of the Contents of 12 Flavonoids in Quzhiqiao from Different Collection Places by HPLC

作　　者：冯敬骞[1] 胡卫南 徐礼萍 李姜言 王思为[4] 宋剑锋 FENG Jingqian;HU Weinan;XU Liping;LI Jiangyan;WANG Siwei;SONG Jianfeng(School of Medicine,Quzhou College of Technology,Zhejiang Quzhou 324000,China;Quzhou Institute for Food and Drug Control,Zhejiang Quzhou 324002,China;Dept.of Pharmacy,Quzhou Hospital of TCM,Zhejiang Quzhou 324022,China;Dept.of Pharmacy,Quzhou Municipal People’s Hospital,Zhejiang Quzhou 324000,China)

机构地区：[1]衢州职业技术学院医学院,浙江衢州324000 [2]衢州市食品药品检验研究院,浙江衢州324002 [3]衢州市中医医院药学部,浙江衢州324022 [4]衢州市人民医院药学部,浙江衢州324000

出　　处：《中国药房》2020年第5期571-575,共5页China Pharmacy

基　　金：国家自然科学基金资助项目(No.81903873);浙江省食品药品监管系统科技计划项目(No.2014006);浙江省衢州市科技计划项目(No.2014Y021)

摘　　要：目的:建立同时测定衢枳壳中12种黄酮类成分含量的方法。方法:采用高效液相色谱法。色谱柱为Agilent Extend C18,流动相为0.1%甲酸水溶液-乙腈溶液(梯度洗脱),流速为1.0 mL/min,柱温为35℃,检测波长为330 nm,进样量为10μL。测定不同采集地的10批衢枳壳样品中12种黄酮类成分(圣草次苷、芸香柚皮苷、柚皮苷、柚皮素、橙皮苷、新橙皮苷、水合橙皮内酯、木犀草素、橙皮内酯、川陈皮素、桔皮素、橙皮油内酯)的含量。结果:圣草次苷、芸香柚皮苷、柚皮苷、柚皮素、橙皮苷、新橙皮苷、水合橙皮内酯、木犀草素、橙皮内酯、川陈皮素、桔皮素、橙皮油内酯检测的质量浓度线性范围分别为1.65~16.51、4.50~45.02、35.41~354.12、4.11~41.12、2.29~22.86、34.96~349.56、1.42~14.15、1.50~15.04、1.83~18.28、1.51~15.08、1.61~16.12、1.28~12.84μg/mL(r均大于0.999 7);检测限分别为0.165 1、0.450 2、3.541 2、0.411 2、0.228 6、3.495 6、0.141 5、0.150 4、0.182 8、0.150 8、0.161 2、0.128 4μg/mL;定量限分别为0.547 8、1.487 4、11.663 3、1.360 3、0.758 3、11.594 9、0.466 3、0.497 1、0.601 2、0.499 9、0.532 3、0.424 6μg/mL;精密度(n=6)、重复性(n=6)、稳定性(24 h,n=7)试验的RSD均小于3%;平均加样回收率分别为99.50%、99.61%、98.18%、98.85%、98.48%、98.50%、98.25%、99.91%、103.13%、98.82%、98.44%、100.29%(RSD=1.49%~2.38%,n=6)。10批不同采集地衢枳壳样品中,上述12个成分的含量分别为1.995 5~2.648 8、4.317 7~5.005 1、33.215 5~34.054 6、3.140 4~3.471 5、3.221 2~3.748 8、42.746 6~44.026 6、0.202 7~0.239 4、0.191 2~0.208 8、0.080 3~0.097 9、0.291 9~0.307 1、0.119 9~0.149 1、0.082 7~0.089 8 mg/g。结论:建立的含量测定方法准确、可靠、简便、高效,可用于同时测定衢枳壳中12个黄酮类成分的含量,并为衢枳壳质量控制标准的建立提供了参考依据。OBJECTIVE:To establish a method for the simultaneous determination of the contents of 12 flavonoids in Quzhiqiao. METHODS:HPLC method was adopted. The determination was performed on Agilent Extend C18 column with mobile phase consisted of 0.1% formic acid-acetonitrile(gradient elution)at the flow rate of 1.0 mL/min. The column temperature was set at 35 ℃. The detection wavelength was set at 330 nm,and sample size was 10 μL. The contents of 12 components(such as eriocitrin,narirutin,naringin,naringenin,hesperidin,neohesperidin,hesperide hydrate,luteolin,hesperide,nobiletin,hesperetin and hesperidolactone)in 10 batches of Quzhiqiao from different collection places were determined. RESULTS:The linear range of eriocitrin,narirutin,naringin,naringenin,hesperidin,neohesperidin,hesperide hydrate,luteolin,hesperide,nobiletin,hesperetin and hesperidolactone were 1.65-16.51,4.50-45.02,35.41-354.12,4.11-41.12,2.29-22.86,34.96-349.56,1.42-14.15,1.50-15.04,1.83-18.28,1.51-15.08,1.61-16.12,1.28-12.84 μg/mL,respectively(all r>0.999 7). The detection limits were 0.165 1,0.450 2,3.541 2,0.411 2,0.228 6,3.495 6,0.141 5,0.150 4,0.182 8,0.150 8,0.161 2,0.128 4 μg/mL,respectively. The limits of quantitation were 0.547 8,1.487 4,11.663 3,1.360 3,0.758 3,11.594 9,0.466 3,0.497 1,0.601 2,0.499 9,0.532 3,0.424 6μg/mL,respectively. RSDs of precision(n=6),reproducibility(n=6)and stability(24 h,n=7)tests were all lower than 3%.The average recoveries were 99.50%,99.61%,98.18%,98.85%,98.48%,98.50%,98.25%,99.91%,103.13%,98.82%,98.44%, 100.29%(RSD=1.49%-2.38%, n=6). The contents of the above 12 components in 10 batches of samples from different collection places were 1.995 5-2.648 8,4.317 7-5.005 1,33.215 5-34.054 6,3.140 4-3.471 5,3.221 2-3.748 8,42.746 6-44.026 6,0.202 7-0.239 4,0.191 2-0.208 8,0.080 3-0.097 9,0.291 9-0.307 1,0.119 9-0.149 1,0.082 7-0.089 8 mg/g. CONCLUSIONS:The method is accurate,reliable,simple and efficient,which can be used to simultaneous determination of the contents of 12 flavonoids in Quzhiqiao,and to provide re

关 键 词：衢枳壳 黄酮类成分 柚皮苷 新橙皮苷 含量测定 高效液相色谱法 

分 类 号：R282[医药卫生—中药学]