色谱

色谱 ›› 2015, Vol. 33 ›› Issue (4): 423-427.DOI: 10.3724/SP.J.1123.2014.12015

• 技术与应用 • 上一篇    下一篇

高效液相色谱法同时测定广陈皮药材中的11种化学成分

叶晓岚1, 宋粉云1, 范国荣2, 毋福海3   

  1. 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
  • 收稿日期:2014-12-10 修回日期:2015-01-19 出版日期:2015-04-08 发布日期:2015-03-30
  • 通讯作者: 毋福海
  • 基金资助:

    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).

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

YE Xiaolan1, SONG Fenyun1, FAN Guorong2, WU Fuhai3   

  1. 1. School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006, China;
    2. Department of Pharmaceutical Analysis, School of Pharmacy, The Second Military Medical University, Shanghai 200433, China;
    3. School of Public Health, Guangdong Pharmaceutical University, Guangzhou 510024, China
  • Received:2014-12-10 Revised:2015-01-19 Online:2015-04-08 Published:2015-03-30

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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, 5 μm)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。

关键词: 非黄酮类化合物, 高效液相色谱法, 广陈皮, 黄酮类化合物

Abstract:

An HPLC method was developed for the simultaneous determination of 11 constituents, 5-hydroxymethyl furfural (5-HMF), vicenin-2, hesperidin, hesperetin, isosinensetin, sinensetin, tetramethyl-O-isoscutellarein (TEOS), nobiletin, 3,5,6,7,8,3',4'-heptamethoxyflavone (HEPTA), tangeretin, 5-demethylnobiletin in Citrus reticulate 'Chachi'. The separation was conducted on a Hanbon Benatach C18 column (250 mm×4.6 mm, 5 μm) with acetonitrile 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 0.0125-1.25 mg/L and 0.0502-4.99 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'.

Key words: Citrus reticulate 'Chachi', flavonoids, high performance liquid chromatography (HPLC), nonflavanoids

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