固相萃取-液相色谱-质谱法超快速测定穿心莲中穿心莲内酯和脱水穿心莲苷

IF 16.4 1区化学 Q1 CHEMISTRY, MULTIDISCIPLINARY

Accounts of Chemical Research Pub Date : 2023-09-04 DOI:10.1556/1326.2023.01156

Zhengming Qian, J. Chen, Qing-Qing Lei, Da Li, Guoying Tan, Juying Xie, Wenqing Li

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引用次数: 0

摘要

采用液相色谱-质谱联用技术建立了穿心莲中穿心莲内酯和脱水穿心莲苷的超快速分析方法。用10 mL 40%（v/v）甲醇，然后用C18固相萃取柱纯化。LC分离在Poroshell 120上进行 EC-C18柱（30 × 2.1 毫米，2.7 μm），用0.5洗脱 mmol L−1乙酸铵水溶液和乙腈（65:35），流速为0.7 mL min−1，并通过质谱法（MS）进行检测。LC-MS分析时间小于1 min.新方法具有良好的线性（r＞0.9900）、精密度和重复性（RSD<2.0%），穿心莲内酯和脱氢穿心莲苷的回收率分别为93.5%（RSD=2.2%）和97.7%（RSD=2.4%）。该方法已成功应用于7批AH样品中穿心莲内酯和脱水穿心莲固体的测定，所有样品中分析物的含量均符合中国药典的相关验收标准（>0.8%），这将有助于提高AH样本测试的效率和降低成本。

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Ultra-rapid determination of andrographolide and dehydroandrographolide in Andrographis Herba by solid phase extraction and liquid chromatography with mass spectrometry

An ultra-rapid analytical method for determination of andrographolide and dehydroandrographolide in Andrographis Herba (AH) was developed by liquid chromatography with mass spectrometry (LC-MS). The sample was ultrasonically extracted with 10 mL 40% (v/v) methanol, and then purified with a C18 solid phase extraction column. The LC separation was performed on a Poroshell 120 EC-C18 column (30 × 2.1 mm, 2.7 μm) and eluted with 0.5 mmol L−1 ammonium acetate aqueous solution and acetonitrile (65:35) at a flow rate of 0.7 mL min−1, and detected by mass spectrometry (MS). The LC-MS analytical time was less than 1 min. The new developed method presented a good linearity (r > 0.9900), precision and repeatability (RSD < 2.0%). The recoveries for andrographolide and dehydroandrographolide were 93.5% (RSD = 2.2%) and 97.7% (RSD = 2.4%), respectively. The developed method was successfully applied in determination of andrographolide and dehydroandrographolide in seven batches of AH samples, and the contents of analytes in all samples were complied with the relative acceptance criteria in Chinese Pharmacopeia (>0.8%). This new developed LC-MS method is an ultra-rapid assay method for AH, which will help to improve the efficiency and reduce the cost of AH sample test.

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来源期刊

Accounts of Chemical Research 化学-化学综合

CiteScore

31.40

自引率

1.10%

发文量

312

审稿时长

2 months

期刊介绍： Accounts of Chemical Research presents short, concise and critical articles offering easy-to-read overviews of basic research and applications in all areas of chemistry and biochemistry. These short reviews focus on research from the author’s own laboratory and are designed to teach the reader about a research project. In addition, Accounts of Chemical Research publishes commentaries that give an informed opinion on a current research problem. Special Issues online are devoted to a single topic of unusual activity and significance. Accounts of Chemical Research replaces the traditional article abstract with an article "Conspectus." These entries synopsize the research affording the reader a closer look at the content and significance of an article. Through this provision of a more detailed description of the article contents, the Conspectus enhances the article's discoverability by search engines and the exposure for the research.