高效液相色谱法同时测定毛两面针药材中5种化学成分含量

Simultaneous Determination of Five Effective Components in Zanthozylum nitidum(Roxb) DC.f. fastuosum How ex Huang by RP-HPLC

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 develop a RP-HPLC method for simultaneous determination of magnoflorine, hesperidin, nitidine chloride, ethoxychelerythrine and toddaloactone in Zanthozylum nitidum （Roxb） DC. f. fastuosum How ex Huang. METHODS The RP-HPLC system consisted of a Diamonsi[ Cls column （4. 6 mm× 250 mm,5 μm） with the mobile phase of aeetonitrile solution-water solution （containing 0. 2% phosphoric acid and 0. 2% triethylamine） for gradient elution. DAD detector was used and the detection wave lengths were 273,283 and 328 nm. The flow rate was 1.0 mL ·min^-1 and the column temperature was 30 ℃. For different con- stituents, external standard method was used with the peak area at the maximum absorption wavelength as the quantitative index. RE- SULTS The liner ranges of magnoflorine, hesperidin, nitidine chloride, ethoxyehelerythrine and toddaloaetone were 0. 095 7 - 1. 339 1 μg （r =0. 999 5） ,0. 318 9 -2. 126 0 μg（r =0. 999 8） ,0. 039 7 -0. 264 8μg（r =0. 999 5） ,0. 100 4 - 1. 004 0μg（r =0. 999 9）, and 0. 108 0 -2. 160 0 μg（r =0. 999 9）, respectively. The average recoveries （n =6） were 100. 2% ,99. 8% ,97.1% ,98.8% and 101.6% （n = 6 ） , respectively. CONCLUSION The method is accurate, simple, rapid, and reproducible for the determination of magnoflorine,hesperidin, nitidine chloride, ethoxychelerythrine and toddaloactone in 2anthoxylum nitidum （Roxb）DC. f. fastuosum How ex Huang. The determination result can be used as a reference for the reasonable medication, quality control and further study of Zanthoxylum nitidum （Roxb） DC. f. fastuosum How ex Huang.