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目的:建立疏风活络丸中伪麻黄碱、麻黄碱、马钱子碱和士的宁的含量测定方法。方法:采用5%氢氧化钠溶液浸润样品后以三氯甲烷于70℃水浴中回流提取,以反相离子对高效液相色谱法测定,采用C18柱(4.6mm×250mm,5μm)分离,柱温30℃;流动相:A为0.01mol.L-1庚烷磺酸钠与0.01mol.L-1磷酸二氢钾等量混合溶液(用磷酸调pH2.8),B为乙腈,梯度洗脱(0min时,A为81%,B为19%;30min时,A为73%,B为27%);流速1.0mL.min-1,检测波长为206nm。结果:4种生物碱成分色谱行为良好,平均回收率(n=6)分别为伪麻黄碱97.36%(RSD=2.1%),麻黄碱97.22%(RSD=2.5%),马钱子碱98.65%(RSD=1.3%),士的宁97.69%(RSD=1.6%)。结论:所建立的方法简单易行,专属性强,准确性好,可用于疏风活络丸中活性兼毒性生物碱类成分的质量控制。
Objective: To establish a method for the determination of pseudoephedrine, ephedrine, strychnine and strychnine in Shufeng Huluo pill. Methods: The samples were infiltrated with 5% sodium hydroxide solution and extracted with chloroform at 70°C in a water bath. The determination was carried out by reversed-phase ion pair high performance liquid chromatography with C18 column (4.6mm×250mm, 5μm). Temperature 30 °C; mobile phase: A is 0.01mol.L-1 sodium heptane sulfonate and 0.01mol.L-1 potassium dihydrogen phosphate equal mixed solution (pH adjusted with phosphoric acid 2.8), B is acetonitrile, gradient washing At 0 min, A was 81% and B was 19%; at 30 min, A was 73% and B was 27%; the flow rate was 1.0 mL.min-1 and the detection wavelength was 206 nm. Results: The chromatographic behaviors of the four alkaloids were good. The average recoveries (n=6) were 97.36% for pseudoephedrine (RSD=2.1%), 97.22% for ephedrine (RSD=2.5%), and 98.65% for brucine (RSD). =1.3%), 97.69% of strychnine (RSD = 1.6%). Conclusion: The established method is simple, easy to use, and has high specificity and accuracy. It can be used for quality control of active and toxic alkaloids in Shufeng Huluo pill.