高效液相色谱法同时测定广陈皮药材中的11种化学成分  

Simultaneous determination of 11 constituents in Citrus reticulate ‘Chachi' by high performance liquid chromatography

作　　者：叶晓岚[1] 宋粉云[1] 范国荣[2] 毋福海[3] 

机构地区：[1]广东药学院药科学院,广东广州510006 [2]第二军医大学药学院药物分析学教研室,上海200433 [3]广东药学院公共卫生学院,广东广州510024

出　　处：《色谱》2015年第4期423-427,共5页Chinese Journal of Chromatography

基　　金：上海市药物(中药)代谢产物研究重点实验室开放基金项目(2012SHDX1002)

摘　　要：采用高效液相色谱法（ HPLC）同时测定了广陈皮药材中5.羟甲基糠醛、维采宁.2、橙皮苷、橙皮素、异甜橙黄酮、甜橙黄酮、异黄芩配基甲醚、川陈皮素、3，5，6，7，8，3′，4′.七甲氧基黄酮、橘皮素及5.去甲川陈皮素11种化学成分的含量。样品经50％（ v／v）甲醇于70℃回流提取。在优化的色谱条件（ Hanbon Benatach C18色谱柱（250 mm ×4.6 mm，5μm）为分离柱，乙腈和0.2％甲酸水溶液为流动相，梯度洗脱，流速1.0 mL／min，柱温25℃，检测波长280 nm）下，提取液中的各成分分离良好，在选定的浓度范围内呈良好的线性关系（ r＞0.998），定量限（ S／N＝10）为0.0502～4.99 mg／L，检出限（ S／N＝3）为0.0125～1.25 mg／L，平均加标回收率（ n＝3）为96.4％～102.4％，相对标准偏差为0.25％～4.01％。该方法准确性高、重复性好，可用于广陈皮的质量控制。An HPLC method was developed for the simultaneous determination of 11 constitu.ents, 5.hydroxymethyl furfural （ 5.HMF ） , vicenin.2, hesperidin, hesperetin, isosinensetin, sinensetin, tetramethyl.O.isoscutellarein （TEOS）, nobiletin, 3,5,6,7,8,3′,4′.heptamethoxy.flavone （ HEPTA） , tangeretin, 5.demethylnobiletin in Citrus reticulate ‘Chachi’ . The separa.tion was conducted on a Hanbon Benatach C18 column （250 mm×4.6 mm, 5μm） with acetoni.trile and 0.2% formic acid as mobile phases with gradient elution. The flow rate was 1.0 mL/min. The detection wavelength was 280 nm. The column temperature was 25℃. The results showed that the correlation coefficients （ r ） between concentration and chromatographic peak area of the 11 constituents were over 0.998 in the selected linear ranges. The limits of detection （ LODs, S/N=3） and limits of quantification （ LOQs, S/N=10） of the 11 constituents were in the range of 0.012 5-1.25 mg/L and 0.050 2-4.99 mg/L, respectively. The average recoveries （ n=3） of the 11 constituents were in the range of 96.4%-102.4% and the RSDs were 0.25%-4.01%. The developed method has been successfully applied for the analysis of eight samples from different cultivation regions in Guangdong Province. This method is simple, accurate and effective for the simultaneous determination of the 11 components, and suitable for the quality control of Citrus reticulate ‘Chachi’ .

关 键 词：高效液相色谱法 黄酮类化合物 非黄酮类化合物 广陈皮 

分 类 号：O658[理学—分析化学]