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目的建立RP-HPLC同时测定17批毛两面针中木兰花碱、橙皮苷、氯化两面针碱、乙氧基白屈菜红碱及毛两面针素的含量。方法以两次不同浓度甲醇溶剂超声法提取药材;采用HPLC优化色谱条件;色谱柱:Diamonsil-C18柱(4.6 mm×250mm,5μm);流动相:乙腈(A)-0.2%磷酸加0.2%三乙胺水溶液(B),梯度洗脱;检测波长:273、283、328nm;流速:1.0 mL.min-1;DAD检测器检测;针对不同组分,选择其最大吸收波长下的峰面积,采用外标法定量;柱温:30℃。结果毛两面针中木兰花碱、橙皮苷、氯化两面针碱、乙氧基白屈菜红碱、毛两面针素的线性范围分别为0.095 7～1.339 1μg(r=0.999 5),0.318 9～2.126 0μg(r=0.999 8),0.039 7～0.264 8μg(r=0.999 5),0.100 4～1.004 0μg(r=0.999 9),0.108 0～2.160 0μg(r=0.999 9);平均加样回收率(n=6)分别为100.2%(RSD 1.5%)、99.8%(RSD 2.4%)、97.1%(RSD 2.0%)、98.8%(RSD 2.2%)、101.6%(RSD 2.6%)。结论该方法简便、快速、准确,重现性好,回收率高,可用于毛两面针药材中5种主要化学成分含量的测定,其结果可为其质量控制、合理用药及进一步研究开发提供参考。
OBJECTIVE To establish a RP-HPLC simultaneous determination of magnaporthelin, hesperidin, nitidine chloride, chelidonine and vinorelbine in 17 batches. Methods The medicinal materials were extracted with two different concentrations of methanol solvent by ultrasonic method. The chromatographic conditions were optimized by HPLC. The chromatographic column was Diamonsil-C18 column (4.6 mm × 250 mm, 5 μm). The mobile phase consisted of acetonitrile-0.2% phosphoric acid and 0.2% (B) gradient elution; detection wavelength: 273,283,328 nm; flow rate: 1.0 mL.min-1; DAD detector detection; for different components, select the maximum absorption wavelength of the peak area, using External standard method; column temperature: 30 ℃. Results The linear range of magnolol, hesperidin, nitidine chloride, ethionine chelidonine and vinblastine was 0.095 7 ~ 1.339 1μg (r = 0.999 5), 0.318 (R = 0.999 5), 0.100 4 ~ 1.004 0μg (r = 0.999 9) and 0.108 0 ~ 2.160 0μg (r = 0.999 9), respectively; The recoveries (n = 6) were 100.2% (RSD 1.5%), 99.8% (RSD 2.4%), 97.1% (RSD 2.0%), 98.8% (RSD 2.2%) and 101.6% (RSD 2.6%) respectively. Conclusion The method is simple, rapid, accurate, reproducible and has high recovery rate. It can be used for the determination of five major chemical constituents in the two-sided needle. The results provide a reference for its quality control, rational drug use and further research and development .