双波长RP-HPLC同时测定骨刺膏渗漉液中马钱子碱、士的宁和乌头碱的含量

Simultaneous Determination of Brucine,Strychnine and Aconitine in Guci Pastes Leachate by Dual Wavelength RP-HPLC

摘要:

目的: 建立RP-HPLC同时测定骨刺膏渗漉液中马钱子碱、士的宁和乌头碱含量的方法.方法: Symmetry C₁₈色谱柱(4.6 mm×250 mm,5 μm),流动相乙腈(A)-水(B)(含0.01 mol ·L^-1磷酸二氢钾溶液,用磷酸调节pH 3)梯度洗脱(0~22 min,11%A;22~23 min,11%~33%A;23~36 min,33%A;36~37 min,33%~11%A;37~40 min,11%A),检测波长为乌头碱235 nm,马钱子碱和士的宁260 nm.结果: 马钱子碱、士的宁和乌头碱的线性范围分别为0.026 4~0.264,0.039 6~0.396,0.016~0.160 μg;平均加样回收率分别为98.44%,98.63%,99.08%,RSD分别为1.84%,1.66%,0.97%;样品中三者的平均质量浓度分别为1.29,1.92,0.79 mg ·L^-1.结论: 该方法操作简便、准确可靠、重复性好,为完善骨刺膏的质量标准提供实验依据.

Abstract:

Objective:To establish a method for determining contents of brucine, strychnine and aconitine in Guci pastes leachate by RP-HPLC. Method: Symmetry C₁₈ column (4.6 mm×250 mm, 5 μm), mobile phase was constituted by acetonitrile(A)-water(B)(containing 0.01 mol · L^-1 potassium dihydrogen phosphate solution, adjusted pH to 3 by phosphoric acid) for gradient elution(0-22 min, 11%A;22-23 min, 11%-33%A;23-36 min, 33%A;36-37 min, 33%-11%A;37-40 min, 11%A) at a flow rate of 1.0 mL · min^-1, detection wavelength was set at 235 nm for aconitine, 260 nm for brucine and strychnine. Result: Linear ranges of brucine, strychnine and aconitine were 0.026 4-0.264, 0.039 6-0.396, 0.016-0.160 μg;their average recoveries were 98.44%, 98.63% and 99.08% with RSD of 1.84%, 1.66% and 0.97%;their average concentrations in samples were 1.29, 1.92, 0.79 mg · L^-1, respectively. Conclusion: This method is simple, accurate and reproducible, it can be provide experimental basis for quality control of Guci pastes.