A sensitive LC-MS/MS method for simultaneous assay of three iridiods in Gardenia jasminoides Ellis
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摘要: 目的 建立同时测定栀子中3种环烯醚萜苷类成分含量的方法。 方法 采用液相色谱-串联质谱（LC-MS/MS）法。色谱条件：Dikma Diamonsil® C18柱（100 mm×4.6 mm，5 μm）；流动相为0.1%乙酸水（A）-0.1%乙酸乙腈（B），梯度洗脱；流速为0.4 ml/min；柱温40℃；进样量2 μl。质谱条件：电喷雾离子化电离源（ESI），正/负离子检测，雾化气流量3 L/min，干燥气流量15 L/min，脱溶剂管温度240℃，加热块温度400℃，碰撞气压力230 kPa，以多反应监测模式（MRM）配对离子方式进行定量，山栀苷、京尼平龙胆双糖苷、栀子苷选择的离子对质荷比分别为m/z 391.10→149.30，m/z 573.40→365.05，m/z 447.30→225.15。 结果 回归方程为：山栀苷Y=243.810X-289.957，r=0.999 9；京尼平龙胆双糖苷Y=137.125X+2 092.76，r=0.999 6；栀子苷Y=2 030.32X+823 213，r=0.999 8；线性范围分别为10.76~2 152 ng/ml、516~4 128 ng/ml、2 000~20 000 ng/ml。精密度、稳定性、重复性和加样回收率试验结果均符合要求。 结论 此方法可快速、准确、灵敏地测定栀子中3种环烯醚萜苷类成分的含量，为栀子的质量控制提供依据。Abstract: Objective To develop a simple, rapid and sensitive method for the determination of major compounds from Gardenia jasminoides Ellis using liquid chromatography tandem mass spectrometry (LC-MS/MS). Methods The analysis was performed on Dikma Diamonsil® C18(100 mm×4.6 mm, 5 μm)column with acetonitrile -0.1% acetic acid and 0.1% acetic acid-water as mobile phase at a rate of 0.4 ml/min.The column temperature was set at 40℃ and the injection volume was 2 μl.Quantification of these compounds was performed by LC-MS/MS with positive or negative ion mode electrospray ionization (ESI) in the multiple reaction monitoring (MRM) mode.Nebulizer gas, 3 L/h; drying gas, 15 L/h; desolvation line (DL) temperature, 240℃; heat block temperature, 300℃; CID, 230 kPa.The mass transition of the precursor/product ions was monitored at m/z 391.10→149.30 for shanzhiside, 573.40→365.05 for genipin-1-gentiobioside, 447.30→225.15 for geniposide. Results The regress equation of shanzhiside, genipin-1-gentiobioside and geniposide were Y=243.810X-289.957, r=0.999 9; Y=137.125X + 2 092.76, r=0.999 6; Y=2 030.32X+823 213, r=0.999 8 in the range of 10.76-215.2 ng/ml; 516-4 128 ng/ml; 2 000-20 000 ng/ml respectively.This validated method has good repeatability, precision, recovery and stability.The results meet the requirements by regulation. Conclusion This method shortened the analysis time and improved efficiency.It assayed the three iridoid glycosides in Gardenia jasminoides Ellis sensitively and precisely.This method can be used for the quality control of Gardenia jasminoides Ellis.
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Key words:
- Gardenia jasminoides Ellis /
- shanzhiside /
- genipin-1-gentiobioside /
- geniposide /
- LC-MS/MS
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