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采用超高效液相色谱-三重四极杆质谱联用技术同时测定酸枣仁汤中六种生物活性成分

Simultaneous Quantification of Six Bioactive Components in Decoction of Ziziphi spinosae Semen Using Ultrahigh Performance Liquid Chromatography Coupled with Triple-Quadrupole Mass Spectrometry.

作者信息

Liu Xiao, Zhu Xiaochai, Zhu Hui, Xie Li, Ma Jia, Xu Yinghui, Zhou Qigang, Wu Zejun, Cai Baochang

机构信息

School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing, China.

Fushun Central Hospital, Fushun, China.

出版信息

J Anal Methods Chem. 2018 Nov 1;2018:8397818. doi: 10.1155/2018/8397818. eCollection 2018.

Abstract

This paper was conducted to develop a method containing ultrahigh performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry for simultaneous quantification of six bioactive components in the decoction of Ziziphi spinosae Semen. Analysis was performed on an Agilent ZORBAX Extend-C column (2.1 × 100 mm, 1.8 m) and eluted with a mobile phase system consisting of acetonitrile and water under a gradient program with a flow rate of 0.3 ml/min. The injection volume was 2 l. Multiple-reaction monitoring scanning detection was employed for quantification with an electrospray ion source in the negative ion mode. All the six compounds showed good linearities ( ≥ 0.9996). The LODs of the six bioactive compounds were 0.039 ng/ml, 0.092 ng/ml, 3.112 ng/ml, 2.131 ng/ml, 0.099 ng/ml, and 0.071 ng/ml for spinosin, 6‴-feruloylspinosin, jujuboside A, jujuboside B, camelliaside B, and betulinic acid, respectively. The LOQs were 0.118 ng/ml, 0.276 ng/ml, 9.336 ng/ml, 6.393 ng/ml, 0.299 ng/ml, and 0.213 ng/ml for spinosin, 6‴-feruloylspinosin, jujuboside A, jujuboside B, camelliaside B, and betulinic acid, respectively. According to our knowledge, it was the first time to establish a method with high efficiency and accuracy for the quantification of six bioactive components in the decoction of Ziziphi spinosae Semen, which would provide references for quality control and evaluation of Ziziphi spinosae Semen.

摘要

本文旨在建立一种超高效液相色谱-三重四极杆串联质谱联用方法,用于同时测定酸枣仁汤中六种生物活性成分的含量。分析采用安捷伦ZORBAX Extend-C柱(2.1×100 mm,1.8 μm),以乙腈和水组成的流动相体系,在梯度洗脱程序下进行洗脱,流速为0.3 ml/min。进样量为2 μl。采用多反应监测扫描检测法进行定量分析,电喷雾离子源采用负离子模式。所有六种化合物均表现出良好的线性关系(r≥0.9996)。六种生物活性化合物的检出限分别为:斯皮诺素0.039 ng/ml、6‴-阿魏酰斯皮诺素0.092 ng/ml、酸枣仁皂苷A 3.112 ng/ml、酸枣仁皂苷B 2.131 ng/ml、山奈酚苷B 0.099 ng/ml、桦木酸0.071 ng/ml。六种生物活性化合物的定量限分别为:斯皮诺素0.118 ng/ml、6‴-阿魏酰斯皮诺素0.276 ng/ml、酸枣仁皂苷A 9.336 ng/ml、酸枣仁皂苷B 6.393 ng/ml、山奈酚苷B 0.299 ng/ml、桦木酸0.213 ng/ml。据我们所知,这是首次建立一种高效、准确的方法用于定量测定酸枣仁汤中六种生物活性成分,可为酸枣仁的质量控制和评价提供参考。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/2cba/6236525/2a2cef7c9687/JAMC2018-8397818.001.jpg

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