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目的建立测定蒙药嘎日迪-13味丸中6种生物碱的含量的高效液相色谱法。方法 Diamonsi I C18色谱柱,以乙腈-四氢呋喃(25∶15)为流动相A,以0.1 mol·L-1醋酸铵溶液为流动相B,梯度洗脱,流速为0.8 m L·min-1,柱温为30℃,检测波长为235 nm,检测专属性、标准曲线与定量下限、精密度与回收率、基质效应和稳定性。结果乌头碱、次乌头碱、新乌头碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰新乌头原碱分别在3.48×10-3~0.17(r=0.999 5),3.24×10-3~0.16(r=0.999 6),6.96×10-3~0.35(r=0.999 5),2.06×10-3~0.10(r=0.999 9),4.04×10-3~0.20(r=0.999 9),6.66×10-3~0.33(r=0.999 9)mg·m L-1呈良好的线性关系,RSD分别为3.56%,1.87%,4.86%,2.74%,3.21%,4.59%,平均回收率分别为101.11%,98.07%,97.81%,99.24%,104.55%,104.84%。结论本方法简便、准确、重复性好,可用于嘎日迪-13味丸中单酯型生物碱和双酯型生物碱的含量测定。
OBJECTIVE To establish a HPLC method for the determination of six alkaloids in Mongolian medicine Jia-di-13. Methods Diamonsi I C18 column was eluted with acetonitrile-tetrahydrofuran (25:15) as mobile phase A and 0.1 mol·L-1 ammonium acetate as mobile phase B at a flow rate of 0.8 m L · min-1. The column temperature was 30 ° C and the detection wavelength was 235 nm. The assay specificity, standard curve and quantification limit, precision and recovery, matrix effect and stability were all obtained. Results The contents of aconitine, hypaconitine, mesaconitine, benzoyl aconitine, benzoyl aconitine and benzoyl aconitine were 3.48 × 10-3 ~ 0.17 r = 0.999 5), 3.24 × 10-3 ~ 0.16 (r = 0.999 6), 6.96 × 10-3 ~ 0.35 (r = 0.999 5), 2.06 × 10-3 ~ 0.10 There was a good linear relationship between 10-3 ~ 0.20 (r = 0.999 9) and 6.66 × 10-3 ~ 0.33 (r = 0.999 9) mg · m L-1 with RSD 3.56%, 1.87%, 4.86%, 2.74 %, 3.21% and 4.59% respectively. The average recoveries were 101.11%, 98.07%, 97.81%, 99.24%, 104.55% and 104.84% respectively. Conclusion The method is simple, accurate and reproducible. It can be used for the determination of monoester alkaloids and diester alkaloids in Gajidi -13 taste pill.