基于UPLC-MS/MS法的参麦颗粒中麦冬掺伪检查方法研究

雷蓉; 刘亚茹; 赵振霞; 刘永利

doi:10.13748/j.cnki.issn1007-7693.20243067

基于UPLC-MS/MS法的参麦颗粒中麦冬掺伪检查方法研究

Study on the Adulteration of Ophiopogonis Radix in Shenmai Granules Based on UPLC-MS/MS

摘要

摘要:
目的建立超高效液相色谱-三重四极杆质谱(UPLC-MS/MS)的参麦颗粒中麦冬掺伪检查方法，考察生产企业是否存在山麦冬掺伪麦冬投料情况。
方法以山麦冬中特征成分短葶山麦冬皂苷C、山麦冬皂苷B为检测指标，分析采用Shimadzu Shim-pack gist C₁₈(2.1 mm×100 mm，2 μm)色谱柱，以0.1%甲酸水溶液-乙腈为流动相等度洗脱，体积流量为 0.3 mL·min⁻¹，柱温 40 ℃。电喷雾正离子源(ESI⁺)扫描，多反应监测(MRM)模式。
结果短葶山麦冬皂苷C、山麦冬皂苷B分别在3.290~315.8 ng·mL⁻¹、 2.390~305.9 ng·mL⁻¹呈良好的线性关系，相关系数均≥0.9996，加样回收率为105.3%、100.6%，精密度、重复性和稳定性的RSD均<3.0%。85批参麦颗粒样品中有8批检出山麦冬皂苷B，检出率为9.4%。
结论建立的方法简便快速、准确性好、专属性强，可用于筛查参麦颗粒中麦冬的掺伪情况。

Abstract:
OBJECTIVE To establish an UPLC-MS/MS method for the adulteration of Ophiopogonis Radix in Shenmai Granules to investigate whether there is a phenomenon of using Liriopes Radix to replace Ophiopogonis Radix in the production enterprise.
METHODS The characteristic components liriope muscari baily saponins C and liriopesides B were used as the detection index of Liriopes Radix. Separation was performed on a Shimadzu Shim-pack gist C₁₈(2.1 mm×100 mm, 2 μm) with a gradient elution of acetonitrile-0.1% formic acid at the flow rate of 0.3 mL·min⁻¹ and a column temperature of 40 ℃. The detection mode was multi reaction monitoring in electrospray positive ion source(ESI⁺).
RESULTS Liriope muscari baily saponins C and liriopesides B showed good linearity in the range of 3.290~315.8 ng·mL⁻¹ and 2.390~305.9 ng·mL⁻¹, with the correlation coefficients ≥0.9996, and the recoveries of 105.3% and 100.6%, and the RSDs of precision, reproducibility, and stability were less than 3.0%. The 85 batches of Shenmai Granules contained 8 batches of Liriopes Radix with the detection rate of 9.4%.
CONCLUSION The established method is simple, rapid, accurate and exclusive, and can be used to screen the adulteration of Ophiopogonis Radix in Shenmai granules.

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