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复方(Wall.)林德液相色谱-串联质谱法质量控制研究。

Study on Quality Control of Compound (Wall.) Lindl. by Liquid Chromatography-Tandem Mass Spectrometry.

机构信息

School of Pharmacy, Fujian Medical University, Fuzhou 350122, China.

出版信息

Molecules. 2022 Jun 27;27(13):4130. doi: 10.3390/molecules27134130.

Abstract

Compound Anoectochilus roxburghii (Wall.) Lindl. (A. roxburghii) oral liquid (CAROL) is a hospital preparation of A. roxburghii and Ganoderma lucidum (G. lucidum), which have hepatoprotective effects. Eight active components (five nucleosides/nucleobases and three triterpenoid acids) in CAROL, A. roxburghii, and G. lucidum were simultaneously detected by high-performance liquid chromatography−tandem mass spectrometry (LC−MS/MS). The multiple reaction monitoring (MRM) mode was applied for the detection of analytes. These eight compounds were separated well within 12 min and quantified using the internal standard working curve method. The method showed good linearity (R2 > 0.9935) and high sensitivity (limit of detection = 0.29 ng/mL). The analyte recovery ranged from 85.07% to 97.50% (relative standard deviation < 3.31%). The content of the target analytes in four batches of CAROL, and the raw materials of G. lucidum and A. roxburghii from the five regions was determined using this method. The contents of guanosine and ganoderic acid A in four batches of oral liquid were high and stabilized and could be recommended as quality markers (Q-marker) for CAROL. Simultaneous qualitative and quantitative analysis of nucleosides and triterpenoid acids in CAROL, A. roxburghii, and G. lucidum by LC−MS/MS based on the MRM model was reported for the first time. The proposed method provides a sensitive, rapid, and reliable approach for the quality control of Chinese medicinal products.

摘要

复方铁皮石斛(Wall.)Lindl.(铁皮石斛)口服液(CAROL)是一种铁皮石斛和灵芝(灵芝)的医院制剂,具有保肝作用。采用高效液相色谱-串联质谱法(LC-MS/MS)同时检测 CAROL、铁皮石斛和灵芝中的 8 种活性成分(5 种核苷/碱基和 3 种三萜酸)。采用多反应监测(MRM)模式检测分析物。这 8 种化合物在 12 分钟内得到很好的分离,并采用内标工作曲线法进行定量。该方法具有良好的线性(R2>0.9935)和高灵敏度(检测限=0.29ng/mL)。分析物回收率在 85.07%至 97.50%之间(相对标准偏差<3.31%)。采用该方法测定了 4 批 CAROL 及灵芝和铁皮石斛 5 个产地原料的目标分析物含量。4 批口服液中鸟苷和灵芝酸 A 的含量较高且稳定,可作为 CAROL 的质量标志物(Q-marker)。首次基于 MRM 模型报道了 LC-MS/MS 同时对 CAROL、铁皮石斛和灵芝中的核苷和三萜酸进行定性和定量分析。该方法为中药质量控制提供了一种灵敏、快速、可靠的方法。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/eea0/9268268/9bc6b82f1fd7/molecules-27-04130-g001.jpg

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