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作 者:余静洁[1] 赵文娜[1] 张新新[1] 苏琪[1] 孙琛[1] 陈琳[1] 何姣[1] 孙文基[1]
机构地区:[1]西北大学陕西省生物医药重点实验室,西安710069
出 处:《西北药学杂志》2012年第5期402-404,共3页Northwest Pharmaceutical Journal
基 金:西北大学研究生创新基金项目(编号:10YZZ34)
摘 要: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.
关 键 词:高效液相色谱法 苦木 3-甲基-铁屎米-2 6-二酮 4-甲氧基-5-羟基铁屎米酮 4 5-二甲氧基-铁屎米酮
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