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超高效液相色谱-线性离子阱-轨道阱质谱联用技术鉴定与测定茵陈清金颗粒的化学成分

Identification and determination of chemical constituents from Yinchen Qingjin granules by ultra high-performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry.

作者信息

Lu Jie, Liang Kun, Chen Ying, Zhao Cheng, Wang Xinhong, An Rui

机构信息

School of Pharmacy, Shanghai University of TCM, Shanghai, P. R. China.

Shanghai Hospital of Integrated Traditional Chinese and Western Medicine, Shanghai University of Traditional Chinese Medicine, Shanghai, P. R. China.

出版信息

J Sep Sci. 2021 Apr;44(7):1324-1344. doi: 10.1002/jssc.202001115. Epub 2021 Jan 25.

Abstract

An ultra high-performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometry method had been used to identify chemical constituents in Yinchen Qingjin Granules. A total of 117 chemical constituents were tentatively identified based on the molecular weight, the mass fragmentation behavior, and the comparison with retention time and accurate mass of reference standards. Meanwhile, an ultra high-performance liquid chromatography coupled with triple quadrupole mass spectrometry method has been developed to evaluate the quality of Yinchen Qingjin Granules through a simultaneous determination of ten components, namely gallic acid, shanzhiside, neochlorogenic acid, chlorogenic acid, caffeic acid, geniposide, liquirition, isoliquirition, glycyrrhizic acid, and rhein. Altogether, content levels of each compound ranged from 0.228 to 8.712 mg/g. At the same time, a hydrophilic interaction liquid chromatography combined with UV for the quantification of sarmentosin in Yinchen Qingjin Granules is presented and its content was from 5.608 to 6.200 mg/g. The linearity, accuracy, and precision of these two validation methods were satisfactory. The both determination methods were successfully used for the analysis of six batches of Yinchen Qingjin Granules samples made in China and could be as suitable analytical method for quality control.

摘要

采用超高效液相色谱-线性离子阱-轨道阱质谱联用方法对茵陈清金颗粒中的化学成分进行鉴定。基于分子量、质谱裂解行为以及与对照品保留时间和精确质量的比较,初步鉴定出117种化学成分。同时,建立了超高效液相色谱-三重四极杆质谱联用方法,通过同时测定没食子酸、山栀苷、新绿原酸、绿原酸、咖啡酸、栀子苷、甘草苷、异甘草苷、甘草酸和大黄酸10种成分来评价茵陈清金颗粒的质量。各化合物含量水平在0.228至8.712mg/g之间。同时,提出了亲水作用液相色谱结合紫外检测法对茵陈清金颗粒中的杠柳苷进行定量分析,其含量为5.608至6.200mg/g。这两种验证方法的线性、准确度和精密度均令人满意。这两种测定方法均成功用于分析6批国产茵陈清金颗粒样品,可作为合适的质量控制分析方法。

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