UPLC-MS/MS同时测定巴戟天中4个环烯醚萜苷的含量

目的：建立UPLC-MS/MS法同时测定巴戟天中4个环烯醚萜苷（水晶兰苷、去乙酰车叶草苷酸、车叶草苷酸和车叶草苷）含量。方法：巴戟天以甲醇回流提取；采用Xbridge BEH C₁₈色谱柱（150 mm×4.6 mm，5 μm），乙腈-0.3%甲酸水为流动相，梯度洗脱；电喷雾离子源，负离子多反应监测模式监测，内标法测定。结果：水晶兰苷、去乙酰车叶草苷酸，车叶草苷酸和车叶草苷质量浓度在0.015~79.65、0.030~96.00、0.042~21.00、0.018~37.50 μg·mL^-1范围内与峰面积呈现良好的线性关系（R²≥0.994 9）；平均加样回收率分别为99.4%、98.5%、98.1%、97.7%，RSD分别为2.3%、2.5%、3.5%、4.1%；不同产地巴戟天中车叶草甘酸和车叶草甘的含量差异较大；结论：该方法可靠，简便，可用于巴戟天中环烯醚萜苷的快速检测。

Objective: To establish a UPLC-MS/MS method for quantitative analysis of monotropein, deacetyl asperulosidic acid, asperulosidic acid and asperuloside in Morindae Officinalis Radix. Methods: Morindae Officinalis Radix was extracted with methanol by reflux extraction. The assay was performed on an Xbridge BEH C₁₈ (150 mm×4.6 mm, 5 μm) column and the sample was eluted with a gradient mobile phase consisting of acetonitrile and 0.3% formic acid. The MS system was operated by using an electrospray ionization (ESI) in the negative ion mode, and the scan mode was in multiple reaction ion monitoring (MRM) mode. Internal standard method was used in the experiment. Results: The linear ranges of monotropein, deacetyl asperulosidic acid, asperulosidic acid and asperuloside were 0.015-79.65 μg·mL^-1, 0.030-96.00 μg·mL^-1, 0.042-21.00 μg·mL^-1 and 0.018-37.50 μg·mL^-1, respectively (R² ≥ 0.994 9). The average recoveries were 99.4%, 98.5%, 98.1% and 97.7% with RSD of 2.3%, 2.5%, 3.5% and 4.1%, respectively. The contents of asperulosidic acid and asperuloside in Morindae Officinalis Radix collected from different areas in China exhibited great variation. Conclusion: The proposed method is reliable and simple, which can be used in rapid detection of iridoid glycosides in Morindae Officinalis Radix.