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目的:建立清热散结胶囊中阿多尼弗林碱的含量检查方法。方法:采用UPLC-MS/MS法,以野百合碱为内标计算浓度。色谱分离采用ACQUITY UPLC BEH C18色谱柱(2.1 mm×50 mm,1.7μm),流动相为0.1%甲酸水溶液(A)-乙腈(B),梯度洗脱(0~2.5 min,6%B;2.5~4 min,6%B→40%B;4~9 min,40%B;9~11 min,40%B→6%B;11~15 min,6%B),流速为0.3 mL·min-1,柱温为30℃,进样量2μL;采用电喷雾离子源,多反应监测模式(MRM)检测。结果:阿多尼弗林碱浓度在0.001~0.046μg·mL-1范围内呈现良好线性关系(r=0.9990),加样回收率为95%~105%,RSD小于2.5%;方法重复性及精密度良好。结论:所建立的方法专属性强,灵敏度高,重复性好,适用于清热散结胶囊中阿多尼弗林碱的检测。
Objective: To establish a method for the determination of adonisifilin in Qingre Sanjie Capsule. Methods: The concentration of monocrotaline was calculated by UPLC-MS / MS. The chromatographic separation was performed on an ACQUITY UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) with a mobile phase of 0.1% formic acid in water (A) -acetonitrile (B), gradient elution (0-2.5 min, 6% B; ~ 4 min, 6% B → 40% B; 4-9 min, 40% B; 9-11 min, 40% B → 6% B; 11-15 min, 6% B) at a flow rate of 0.3 mL · min -1, the column temperature was 30 ℃, and the injection volume was 2μL. Electrospray ionization (ESI) and multi-reaction monitoring (MRM) were used. Results: The linear range of ADNF was 0.001 ~ 0.046μg · mL-1 (r = 0.9990), the recoveries were 95% -105% and the RSD was less than 2.5%. The repeatability and Good precision. Conclusion: The established method has the advantages of high specificity, high sensitivity and good reproducibility. It is suitable for the determination of adoniflin base in Qingre Sanjie Capsule.