铁棒锤中3种双酯生物碱的含量测定

目的为铁棒锤的合理使用及质量控制提供依据。方法色谱柱:Diamonsil C_(18)柱(250mm×4.6mm,5μm);流动相:以乙腈-四氢呋喃(25∶15)为流动相A,以0.1mol·L~(-1)醋酸铵溶液(每1 000mL加冰乙酸0.5mL)为流动相B,梯度洗脱;流速:1.0mL·min~(-1);检测波长:235nm。结果在此色谱条件下,3种双酯型生物碱可以完全分离,乌头碱、次乌头碱、新乌头碱的线性范围分别为:0.13~1.33μg(r=0.999 0),0.34~3.41μg(r=0.998 2)和0.34~3.41μg(r=0.998 1),回收率分别为97.0%(RSD=1.290%),97.0%(RSD=1.174%)和96.3%(RSD=1.521%)。结论该方法操作简便,结果准确可靠,重复性好,能用于铁棒锤中3种双酯型生物碱的含量测定。甘肃产铁棒锤中乌头碱、次乌头碱、新乌头碱的平均含量分别为0.183%,0.012%和0.055%,酯碱含量高,临床使用时应减少用量或炮制后使用。

Simultaneous determination of 3 diester diterpenoid alkaloids in Radix Aconiti Pendulum

Objective To provide a basis for the rational use and the quality control of Radix Aconiti Pendulum.Methods The assay was performed on a Diamonsil C18(250 mm×4.6 mm,5 μm)column by gradient elution using mobile phase made of A and B at a flow of 1.0 mL·min-1,and the mobile phase A consisted of acetonitrile and tetrahydrofuran (25∶15),and the mobile phase B consisted of 0.1 mol·L-1ammonium acetate solution (1 000 mL solution mixed 0.5 mL glacial acetic acid);the eluent was monitored by a UV detector at 235 nm.Results The three diester diterpenoid alkaloids were eluted preferably under the chromatographic condition.Aconitine showed a good linear relationship in the range of 0.13-1.33 μg (r=0.999 0),the average recovery was 97.0% and RSD was 1.290%;Hypaconitine showed a good linear relationship in the range of 0.34-3.41 μg (r=0.998 2),the average recovery was 97.0% and RSD was 1.174%;Mesaconitine showed a good linear relationship in the range of 0.34-3.41 μg (r=0.998 1),the average recovery was 96.3% and RSD was 1.521%.Conclusion The method of identification and quantification is simple,reliable,and reproducible,and it can be used effectively for the quality control of Radix Aconiti Pendulum.The average contents of aconitine,hypaconitine and mesaconitine in Radix Aconiti Pendulum from Gansu Province were 0.183%,0.012% and 0.055%, respectively.Since the total content of 3 diester diterpenoid alkaloids was high,so it is advised to reduce the dosage or be processed before utilized in clinical.