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采用超高效液相色谱- Q Exactive 混合四极杆轨道阱高分辨精确质量质谱法对益心舒片进行定性和定量测定。

Qualitative and quantitative determination of YiXinShu Tablet using ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry.

机构信息

Department of Pharmacy, The First Affiliated Hospital of Zhengzhou University, Zhengzhou, P. R. China.

College of Medicine, Henan Polytechnic University, Jiaozuo, P. R. China.

出版信息

J Sep Sci. 2017 Nov;40(22):4453-4466. doi: 10.1002/jssc.201700619.

DOI:10.1002/jssc.201700619
PMID:28837751
Abstract

To clarify and quantify the chemical profile of YiXinShu Tablet rapidly, a feasible and accurate strategy was developed by applying ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry. A total of 105 components were identified, including 25 phenanthraquinones, 11 lactones, 19 lignans, 24 acids, and 26 other compounds. Among them, 26 major compounds were unambiguously detected by comparing with reference standards. And 19 of these compounds in three batches of YiXinShu Tablet were selected for quantitative determination. (Z)-Ligustilide, salvianic acid A, salvianolic acid A, salvianolic acid B, and rosmarinic acid were abundant in these three batches with contents over 1 mg/g. The established analysis methods were examined to be accurate and feasible. The results show that the ultra high performance liquid chromatography with Q Exactive hybrid quadrupole orbitrap high-resolution accurate mass spectrometry method has a powerful qualitative ability and promising quantitative application.

摘要

为了快速阐明和量化益心舒片的化学成分特征,应用超高效液相色谱- Q Exactive 杂交四极杆轨道阱高分辨精确质量质谱法建立了一种可行且准确的策略。共鉴定出 105 个成分,包括 25 个蒽醌类化合物、11 个内酯类化合物、19 个木脂素类化合物、24 个酸类化合物和 26 个其他化合物。其中,通过与对照品比较,明确检测到 26 种主要化合物。选择 19 种化合物在三批益心舒片中进行定量测定。(Z)-藁本内酯、丹酚酸 A、丹酚酸 A、丹酚酸 B 和迷迭香酸在这三批样品中含量丰富,均超过 1mg/g。所建立的分析方法被证明是准确和可行的。结果表明,超高效液相色谱- Q Exactive 杂交四极杆轨道阱高分辨精确质量质谱法具有强大的定性能力和有前途的定量应用。

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