建立了简便、快速、灵敏、环保的LC-MS/MS同时测定10种冬虫夏草中游离虫草素和异虫草素含量的方法

IF 1.7 4区化学 Q3 CHEMISTRY, ANALYTICAL

Acta Chromatographica Pub Date : 2022-11-15 DOI:10.1556/1326.2022.01094

Wenqing Li, Z. Qian, Yuansheng Zou, Guoying Tan, Wenjia Li, Qing-Qing Lei, Run-feng Li, Dongming Lan

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引用次数: 1

摘要

建立了一种简便、快速、灵敏、环保的液相色谱-串联质谱法（LC-MS/MS）同时测定10种虫草样品中游离虫草素（3′-脱氧腺苷）和异虫草素（2′-脱氧腺苷酸）的方法。样品通过75℃的超声波提取制备 °C持续30 min，用沸水作为提取溶剂。LC分离在Agilent poroshell 120 SB Aq C18柱（3.0 × 50 毫米，2.7 μm）与环保型流动相（含0.2%乙酸的2%乙醇）以0.6 mL min−1的流速在等度模式下进行检测，并通过MS/MS在阳性模式下进行多重反应监测（MRM）检测。该方法具有良好的线性（r＞0.9990）、灵敏度（LOD＝0.04） pg，LOQ=0.1 pg）、精密度（RSD≤3.8%）和稳定性（RSD≤3.6%）。该方法的回收率为94.4–109.5%（RSD≤5.5%）。与已报道的方法相比，该方法快速（分析时间小于35%）、灵敏（5倍以上）、环保（小于10 μL有害有机溶剂）。采用该方法对10个不同品种（40批次）的冬虫夏草样品进行了检测。虫草素仅在冬虫夏草和C.millitaris子实体中发现，在冬虫虫夏草等6个虫草样品中检测到异虫草素。所开发的方法将是一种改进的虫草样品质量评价方法。

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A simple, rapid, sensitive and eco-friendly LC-MS/MS method for simultaneous determination of free cordycepin and isocordycepin in 10 different kinds of Cordyceps

A simple, rapid, sensitive and eco-friendly liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for simultaneous determination of free cordycepin (3′-deoxyadenosine) and isocordycepin (2′-deoxyadenosine) in 10 kinds of Cordyceps samples. The samples were prepared by ultrasonic extraction at 75 °C for 30 min with boiling water as the extraction solvent. The LC separation was performed on an Agilent poroshell 120 SB-Aq C18 column (3.0 × 50 mm, 2.7 μm) in isocratic mode with an eco-friendly mobile phase (2% ethanol containing 0.2% acetic acid) at a flow rate of 0.6 mL min−1, and detected by MS/MS in positive mode with multiple reaction monitoring (MRM). The developed method showed good linearity (r > 0.9990), sensitivity (LODs = 0.04 pg, LOQ = 0.1 pg), precision (RSD ≤ 3.8%) and stability (RSD ≤ 3.6%). The recoveries of developed method were 94.4–109.5% (RSD ≤ 5.5%). Compared with reported methods, the current method was rapid (less than 35% analytical time), sensitive (more than 5 folds), and eco-friendly (less than 10 μL harmful organic solvent). 10 different kinds of Cordyceps samples (40 batches) were tested by the developed method. Codycepin was only found in Cordyceps millitaris and C. millitaris fruiting body, and isocordycepin was detected in Cordyceps sinensis and other 6 Cordyceps samples. The developed method would be an improved method for the quality evaluation of Cordyceps samples.

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来源期刊

Acta Chromatographica 化学-分析化学

CiteScore

4.00

自引率

0.00%

发文量

审稿时长

2.3 months

期刊介绍： Acta Chromatographica Open Access Acta Chromatographica publishes peer-reviewed scientific articles on every field of chromatography, including theory of chromatography; progress in synthesis and characterization of new stationary phases; chromatography of organic, inorganic and complex compounds; enantioseparation and chromatography of chiral compounds; applications of chromatography in biology, pharmacy, medicine, and food analysis; environmental applications of chromatography; analytical and physico-chemical aspects of sample preparation for chromatography; hyphenated and combined techniques; chemometrics and its applications in separation science.