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采用气相色谱-质谱联用和超高效液相色谱法对正天丸挥发性成分进行定性和定量分析

Qualitative and Quantitative Analysis of Volatile Components of Zhengtian Pills Using Gas Chromatography Mass Spectrometry and Ultra-High Performance Liquid Chromatography.

作者信息

Liu Cui-Ting, Zhang Min, Yan Ping, Liu Hai-Chan, Liu Xing-Yun, Zhan Ruo-Ting

机构信息

Research Center of Chinese Medicinal Resource Science and Engineering, Key Laboratory of Chinese Medicinal Resources from Lingnan of Ministry of Education, Joint Laboratory of National Engineering Research Center for the Pharmaceutics of Traditional Chinese Medicines, Guangzhou University of Traditional Chinese Medicine, Guangzhou, Guangdong 510006, China.

School of Chinese Herbal Medicine, Guangzhou University of Chinese Medicine, Guangzhou, Guangdong 510006, China.

出版信息

J Anal Methods Chem. 2016;2016:1206391. doi: 10.1155/2016/1206391. Epub 2016 Jan 20.

Abstract

Zhengtian pills (ZTPs) are traditional Chinese medicine (TCM) which have been commonly used to treat headaches. Volatile components of ZTPs extracted by ethyl acetate with an ultrasonic method were analyzed by gas chromatography mass spectrometry (GC-MS). Twenty-two components were identified, accounting for 78.884% of the total components of volatile oil. The three main volatile components including protocatechuic acid, ferulic acid, and ligustilide were simultaneously determined using ultra-high performance liquid chromatography coupled with diode array detection (UHPLC-DAD). Baseline separation was achieved on an XB-C18 column with linear gradient elution of methanol-0.2% acetic acid aqueous solution. The UHPLC-DAD method provided good linearity (R (2) ≥ 0.9992), precision (RSD < 3%), accuracy (100.68-102.69%), and robustness. The UHPLC-DAD/GC-MS method was successfully utilized to analyze volatile components, protocatechuic acid, ferulic acid, and ligustilide, in 13 batches of ZTPs, which is suitable for discrimination and quality assessment of ZTPs.

摘要

正天丸是常用于治疗头痛的中药。采用超声法用乙酸乙酯提取正天丸的挥发性成分,并用气相色谱 - 质谱联用仪(GC - MS)进行分析。鉴定出22种成分,占挥发油总成分的78.884%。采用超高效液相色谱 - 二极管阵列检测法(UHPLC - DAD)同时测定原儿茶酸、阿魏酸和藁本内酯这三种主要挥发性成分。在XB - C18柱上以甲醇 - 0.2%乙酸水溶液进行线性梯度洗脱实现了基线分离。UHPLC - DAD法具有良好的线性(R (2)≥0.9992)、精密度(RSD < 3%)、准确度(100.68 - 102.69%)和耐用性。UHPLC - DAD/GC - MS法成功用于分析13批正天丸中的挥发性成分、原儿茶酸、阿魏酸和藁本内酯,适用于正天丸的鉴别和质量评价。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ade0/4745273/0134e6d6df87/JAMC2016-1206391.001.jpg

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