液相色谱-串联质谱法测定蓝芩口服液中16种化学成分的含量

Simultaneous determination of sixteen components in Lanqin oral solution by LC-MS/MS

目的 建立同时测定蓝芩口服液中16种化学成分含量的方法。方法 采用液相色谱-串联质谱法(LC-MS/MS)。Fortis Xi C_(18)柱(100 mm×2.1 mm,1.7μm);流动相为0.1%甲酸水溶液(A)-乙腈(B);梯度洗脱;流速:0.3 mL/min;进样量:2μL;柱温:40℃;质谱采用电喷雾离子源(ESI)正负离子模式,多反应监测(MRM)方式进行测定。结果 蓝芩口服液中汉黄芩苷、黄芩苷、异牡荆苷、栀子苷、巴马汀、黄柏碱、木兰花碱、小檗碱、鸟苷、汉黄芩素、黄芩素、腺苷、胞苷、表告依春、山栀苷和绿原酸等16个成分浓度分别在所考察的浓度范围内与峰面积呈良好的线性关系(r>0.999 0);精密度、稳定性、重复性RSD均<2.5%,加样回收率(n=9)在91.7%~108.3%范围内,RSD<3.5%。结论 所建立的LC-MS/MS方法简便、可靠、选择性好、灵敏度高,可用于蓝芩口服液的质量控制。

Objective To develop a simple,rapid and sensitive method for the determination of sixteen compounds in Lanqin oral so⁃lution.Methods The method was LC-MS/MS.The analysis was performed on Fortis Xi C_(18)(100 mm×2.1 mm,1.7μm)column with 0.1%formic acid-water and acetonitrile as mobile phase at a rate of 0.3 mL/min.The column temperature was set at 40℃and the injec⁃tion volume was 2μL.Ectrospray ionization(ESI)interface and multiple reaction monitoring(MRM)were used.Results All calibration curves of sixteen components(wogonoside,baicalin,isovitexin,geniposide,palmatine,phellodendrine,magnoflorine,berberine,guano⁃sine,wogonin,baicalein,adenosine,cytidine,epigoitrin,shanzhiside,chlorogenic acid)were linear(r>0.9990)over the tested ranges.The repeatability,precision and stability with RSD<2.5%.The average recoveries(n=9)ranged from 91.7%to 108.3%with RSD<3.5%.The results of the sixteen compounds of samples all met the requirements of the national standards,but the content of the sixteen components between batches varied greatly.Conclution The established LC-MS/MS method is convenient,reliable,with good selec⁃tivity and high sensitivity,which can be used for the quality control of Lanqin oral solution.