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采用亲水作用色谱/飞行时间质谱和反相液相色谱/飞行时间质谱联用技术鉴定冠心宁注射液中的多种成分。

Identification of multiple components in Guanxinning injection using hydrophilic interaction liquid chromatography/time-of-flight mass spectrometry and reversed-phase liquid chromatography/time-of-flight mass spectrometry.

机构信息

Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, Shanghai 200433, China.

出版信息

Rapid Commun Mass Spectrom. 2011 Jun 15;25(11):1661-74. doi: 10.1002/rcm.5003.

DOI:10.1002/rcm.5003
PMID:21594942
Abstract

An approach for the identification of multiple components in traditional Chinese medicine injections (TCMIs) using a combination of hydrophilic interaction chromatography (HILIC) and reversed-phase liquid chromatography (RPLC) coupled with time-of-flight mass spectrometry (TOFMS) was developed for the quality control of Guanxinning injection (GXNI), a widely used TCMI, composed of Salvia miltiorrhiza and Ligusticum Chuanxiong. A total of 50 compounds from five compound classes, including saccharides, amino acids, organic acids, phenolic acids and phthalides, were identified or tentatively characterized on the basis of accurate mass measurements and subsequent TOFMS product ions. Six groups of isomers of phenolic acids and saccharides were tentatively distinguished. It was observed that the ESI-TOFMS fragmentation behavior of phthalides was different in negative and positive ion mode, and the fragmentation pathways were tentatively elucidated using structurally-relevant product ions. Several highly polar constituents were characterized for the first time from GXNI by HILIC/TOFMS. In addition, all the constituents identified from GXNI were further assigned in the two individual crude drugs. The integrated strategy has provided a powerful approach for the separation and identification of the multiple components in GXNI, and it has also assisted in the establishment of methods for the comprehensive safety and quality evaluation of TCMIs.

摘要

建立了一种亲水作用色谱(HILIC)和反相液相色谱(RPLC)与飞行时间质谱(TOFMS)联用的方法,用于鉴定中药注射液(TCMIs)中的多种成分,以控制广泛使用的丹参川芎嗪注射液(GXNI)的质量。该注射液由丹参和川芎组成。基于精确质量测量和随后的 TOFMS 产物离子,从五个化合物类别中鉴定或暂定鉴定了 50 种化合物,包括糖、氨基酸、有机酸、酚酸和苯酞。暂定区分了 6 组酚酸和糖的异构体。观察到苯酞在正负离子模式下的 ESI-TOFMS 碎裂行为不同,并使用结构相关的产物离子初步阐明了碎裂途径。首次通过 HILIC/TOFMS 从 GXNI 中鉴定出几种高极性成分。此外,从 GXNI 中鉴定出的所有成分都进一步在两种原料药中进行了归属。综合策略为 GXNI 中多种成分的分离和鉴定提供了有力的方法,也有助于建立中药注射液全面安全性和质量评价的方法。

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