HPLC法测定不同产地苦木药材中3种生物碱

Determination of three alkaloids in Picrasma quassioidesfrom different producing areas by HPLC

目的建立苦木药材中4,5-二甲氧基-铁屎米酮、4-甲氧基-5-羟基铁屎米酮和3-甲基-铁屎米-2,6-二酮的HPLC测定方法,为苦木的质量分析和评价建立了分析方法。方法采用高效液相法,色谱柱为Welchrom C18色谱柱(250mm×4.6mm,5μm);以乙腈(A)-1mL.L-1乙酸水(B)为流动相;梯度洗脱,流速1.0mL.min-1;检测波长254nm;柱温30℃。结果 3-甲基-铁屎米-2,6-二酮,4-甲氧基-5-羟基铁屎米酮和4,5-二甲氧基-铁屎米酮线性范围分别为5.5～38.5(r=0.999 8),19.8～138.6(r=0.999 7)和8.3～58.1μg.mL-1(r=0.999 9);平均加样回收率分别为99.4%,100.7%和100.5%。结论该方法简便、易行,稳定、可靠,为苦木药材的质量分析、评价和进一步研究开发提供参考。

Objective To establish a method for determination of three alkaloids： 4, 5-dimethoxycanthin-6-dione; 4-methoxy-5-hydroxycanthin-6-dione;3-methylcanthin-2,6-dione in Picrasma quassioides, and to provide a basis for the quality and evaluation of Picrasma quassioides. Methods The determination was carried out with a Welchrom C18 column（250mm×4.6mm,5μm）. The mobile phase consisted of acetonitrile （A）-1 mL·L^-1 acetic acid （B） ,gradient elution,at a flow rate of 1.0 mL·min^-1. The detection wavelength was 254 nm,and the column temperature was 30℃. Results The calibration curves were linear in the ranges of 5.5-38.5 μmL·L^-1 for 3-methylcanthin-2,6-dione （r=0. 999 8 ）, 19.8-138.6 μmL·L^-1 for 4-methoxy-5-hydro-xycanthin-6- dione（r= 0. 999 7） and 8.3-58. μmL·L^-1 for 4,5-dimethoxycanthin-6-dione （r=0. 999 9）. The average recoveries were 99.40%, 100.7% and 100.5% ,respectively. Conclusion The method is simple, feasible, stable and reliable,which can provide the basis for the quality and evaluation,meanwhile offer a reference for the further research and development of Picrasma quassioides.