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[摘要]
目的 建立高效液相色谱-串联质谱法(HPLC-MS/MS)测定山药中尿囊素的量.方法 采用Agilent Eclipse Plus C18色谱柱(100 mm×4.6 mm,3.5 μm),以乙腈-水(90:10)为流动相,体积流量0.3 mL/min,柱温为30 ℃;采用电喷雾负模式电离(ESI-),多反应监测扫描模式(MRM)进行定量分析,选定的母离子是m/z 156.9,定量子离子是m/z 96.7.结果 尿囊素在0.12~6.0 μg/mL范围内线性关系良好(r=0.998 5),平均加标回收率为101%(n=6),RSD为3.2%.结论 本方法灵敏、准确、专属性强,能准确有效地测定出山药中尿囊素的量.
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[Abstract]
Objective To establish an HPLC-MS/MS method for determination of allantoin in Dioscoreae Rhizoma. Methods Determination of LC system used Agilent Eclipse Plus C18 (100 mm × 4.6 mm, 3.5 μm) column and acetonitrile-water (90:10) as mobile phase in linear gradient condition. The flow rate was 0.3 mL/min. The mass spectrometer was operated under the negative ion mode with ESI source. MRM (precursor ion of m/z 156.9 and product ion of m/z 96.7) was used to qualify allantoin. Results The linear range of the component was 0.12—6.0 μg/mL, r=0.998 5; The average recovery was 101%, and the RSD was 3.2%. Conclusion The method is sensitive, reliable, and accurate, and can be applied in the quality control of Dioscoreae Rhizoma.
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