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超快速液相色谱-四极杆飞行时间质谱联用鉴定中药复方参松养心胶囊中的多种成分

Identification of multiple constituents in Chinese medicinal prescription Shensong Yangxin capsule by ultra-fast liquid chromatography combined with quadrupole time-of-flight mass spectrometry.

作者信息

Liu Minyan, Zhao Shaohua, Wang Yufeng, Liu Ting, Li Song, Wang Hongtao, Tu Pengfei

机构信息

State Key Laboratory of Natural and Biomimetic Drugs, School of Pharmaceutical Science, Peking University, 38 Xueyuan Road, Beijing 100191, China Shijiazhuang Yiling Pharmaceutical Co., Ltd, Shijiazhuang 050035, China.

Shijiazhuang Yiling Pharmaceutical Co., Ltd, Shijiazhuang 050035, China.

出版信息

J Chromatogr Sci. 2015 Feb;53(2):240-52. doi: 10.1093/chromsci/bmu047. Epub 2014 May 28.

Abstract

A practical method using ultra-fast liquid chromatography in tandem with quadrupole time-of-flight mass spectrometry combined with dynamic background subtraction technology was developed for the rapid separation and identification of the complicated constituents in the Shensong Yangxin capsule (SSYX). The chromatographic separation was performed on a C18 column (2.1 × 100 mm, 2.6 μm) with a gradient elution program using methanol and 0.1% formic acid aqueous solution as the mobile phase at a flow rate of 0.4 mL min(-1). Accurate mass measurements of the molecular ions in the full scan and the characteristic fragment ions triggered by information-dependent acquisition provided reliable identification criteria. Thus, 99 compounds, including saponins, phenolic acids, tanshinones, lignans, terpenoids, alkaloids and flavonoids, were unambiguously or tentatively identified in 40 min by comparing their retention times and accurate mass measurements for each molecular ion and its subsequent fragment ions with those of authentic standards or literature data. Simultaneously, all the compounds were further assigned to the individual raw materials. In conclusion, these results will provide a basis for quality control and further study of SSYX, and the proposed technique based on high-resolution mass spectrometry would be expected to be adaptable to the analysis of complicated constituents in various complex matrices.

摘要

建立了一种结合超快速液相色谱-四极杆飞行时间质谱联用技术与动态背景扣除技术的实用方法,用于快速分离和鉴定参松养心胶囊(SSYX)中的复杂成分。色谱分离在C18柱(2.1×100 mm,2.6μm)上进行,采用梯度洗脱程序,以甲醇和0.1%甲酸水溶液为流动相,流速为0.4 mL min(-1)。全扫描中分子离子的精确质量测量以及信息依赖采集触发的特征碎片离子提供了可靠的鉴定标准。因此,通过将每种分子离子及其后续碎片离子的保留时间和精确质量测量值与标准品或文献数据进行比较,在40分钟内明确或初步鉴定出99种化合物,包括皂苷、酚酸、丹参酮、木脂素、萜类、生物碱和黄酮类。同时,所有化合物进一步归属于各个原料。总之,这些结果将为SSYX的质量控制和进一步研究提供依据,并且基于高分辨率质谱的所提出技术有望适用于各种复杂基质中复杂成分的分析。

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