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目的:建立UPLC-MS/MS法测定南方山荷叶与八角莲中鬼臼毒素-4-O-葡萄糖苷、4’-去甲鬼臼毒素、鬼臼毒素、4-去氧鬼臼毒素的含量。方法:采用Waters BEH C18色谱柱(100 mm×2.1 mm,1.7μm),以甲醇-0.1%甲酸溶液(10 mmol/L乙酸铵)为流动相进行梯度洗脱;流速为0.3 m L/min;柱温为30℃;质谱条件:采用正离子的模式,以MRM配对离子方式进行定量分析。结果:4种木脂素类成分均在4 min内出峰且分离良好,鬼臼毒素-4-O-葡萄糖苷、4’-去甲鬼臼毒素、鬼臼毒素、4-去氧鬼臼毒素分别在156.25~10 000 ng/m L、40.63~2 600 ng/m L、159.38~10 200 ng/m L、8.13~520 ng/m L范围内线性关系良好(r>0.998),平均加样回收率为98.2%~105.0%,RSD均小于4.2%(n=3)。结论:该方法专属性强、快速灵敏,可用于南方山荷叶与八角莲中多种成分含量的测定。
OBJECTIVE: To establish a UPLC-MS / MS method for the determination of podophyllotoxin-4-O-glucoside, 4’-detoxypodophyllotoxin, podophyllotoxin, 4-deoxypodophyllotoxin content. Methods: The gradient elution was performed on a Waters BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with methanol-0.1% formic acid (10 mmol / L ammonium acetate) as the mobile phase at a flow rate of 0.3 m L / min. The column temperature was 30 ℃. Mass spectrometry conditions: positive ion mode was used to quantitatively analyze MRM ion pair. Results: Four kinds of lignan components peaked and separated well within 4 min. The contents of podophyllotoxin-4-O-glucoside, 4’-demethoxypodophyllotoxin, podophyllotoxin, The toxins had a good linear relationship (r> 0.998) in the range of 156.25-10 000 ng / m L, 40.63-2 600 ng / m L, 159.38-10,200 ng / m L and 8.13-520 ng / The average recoveries ranged from 98.2% to 105.0% with RSDs less than 4.2% (n = 3). Conclusion: The method is specific, rapid and sensitive, and can be used for the determination of the contents of many components in the leaves of lotus nigra and.