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目的:建立高效液相色谱-电喷雾串联质谱联用技术(HPLC-ESI-MS/MS)法同时测定金线风中7种成分含量的方法。方法:采用Waters CORTECS C_(18)(2.1mm×100mm,1.6μm)色谱柱,乙腈-0.1%甲酸水溶液为流动相梯度洗脱,样品经电喷雾电离离子源(ESI)正离子化后,通过安捷伦三重四级杆串联质谱仪,采用选择多反应监测(MRM)对金线风进行分析。结果:木兰花碱、β-蜕皮甾酮、轮环藤碱、非洲防己碱、药根碱、巴马亭红碱、掌叶防己碱在一定范围内具有较好的线性关系,R~2≥0.9997,精密度、重复性和稳定性的RSD<5%,加样回收率均在96.7%-104.8%之间。结论:本实验建立的方法准确度和灵敏度高,专属性好,可作为金线风的质量控制方法。
OBJECTIVE: To establish a method for simultaneous determination of seven constituents in the air and wind by high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS / MS). METHODS: Waters CORTECS C 18 (2.1 mm × 100 mm, 1.6 μm) column and acetonitrile-0.1% formic acid aqueous solution were used as the mobile phases for gradient elution. The samples were ionized by electrospray ionization ionization (ESI) Agilent triple quadrupole tandem mass spectrometer, using a choice of multiple reaction monitoring (MRM) to analyze the gold wire wind. Results: Magnolifine, β-ecdysterone, cycloiodine, tetrandrine, jatrorrhizine, palmatine and palmatine had a good linear relationship in a certain range. R 2> 0.9997, RSD <5% for precision, repeatability and stability, recoveries were all between 96.7% and 104.8%. Conclusion: The method established in this experiment has the advantages of high accuracy and sensitivity, good specificity and can be used as quality control method of wind and gold wire.