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Rapid determination of amino acids without derivatization using hydrophilic interaction ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry

Rapid determination of amino acids without derivatization us...

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中华中医药学会中药分析分会第五届学术交流会

作者： Sheng Guo,Jin-ao Duan~*,Dawei Qian,Yuping Tang,Yefei Qian,Dawei Wu,Shulan Su,Erxin Shang Jiangsu Key Laboratory for High Technology Research of TCM Formulae,Nanjing University of Chinese Medicine,Nanjing 210046,PR. China

A novel hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry (HIL1C-MS/MS) method was developed for the simultaneous determination of 23 free amino acids without derivatization.The method was performed on an ultra-high performance liquid chromatography(UHPLC) separation system coupled with electrospray ionization mass spectrometry on a triple quadrupole mass spectrometer (TQ-MS),operating in positive ionization mode.Sufficient separation of the 23 underivatized amino acids was achieved on an Acquity BEH Amide column(2.1 mm×100 mm,1.7μm) in a single run of 12 min at a flow rate of 0.4 mL min.The limits of detection were in the range from 0.17 to 77.75 ng mL.All the analytes were quantified directly from biological extracts without any kind of derivatization,which avoided the laborious and time-consuming of derivatization procedures used by the traditional method.Also,the more polar compounds were separated without utilization of perfluorinated acids as ion-pairing reagents which was not suggested for ESI source. Then,the method was applied for the analysis of the free amino acids in 46 batches of Ziziphus jujuba fruits which comprised 39 cultivars from 26 cultivation regions.Multivariate statistical analysis was also used to investigate the differences in free amino acid profiles among the samples.This study showed that HILIC-UHPLC-TQ-MS is an effective technique to analyze underivatized amino acids in the biological samples.

关键词： Amino acid Ziziphus jujuba Hydrophilic interaction chromatography Ultra-high performance liquid chromatography triple quadrupole mass spectrometry

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Characterization and quantitation of aristolochic acid analogs in different parts of Aristolochiae Fructus, using UHPLC-Q/TOF-MS and UHPLC-Qq Q-MS

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Chinese Journal of Natural Medicines 2017年第5期15卷 392-400页

作者： MAO Wen-Wen GAO Wen LIANG Zhi-Tao LI Ping ZHAO Zhong-Zhen LI Hui-Jun State Key Laboratory of Natural Medicines China Pharmaceutical University School of Chinese Medicine Hong Kong Baptist University

Aristolochiae Fructus, a Chinese herbal medicine derived from the fruit of Aristolochia contorta Bge., contains nephrotoxic aristolochic acid analogues(AAAs). According to ancient medical texts, various medicinal parts of the fruit of A. contorta were ever used. In order to reveal which part could be safely and effectively used, it is necessary to analyze the chemical profiles of different medicinal parts. Herein we compared the chemical compositions and determined aristolochic acid I(AA-I) and aristolochic acid II(AA-II) in the four parts viz. outer pericarp, inner pericarp, septum, and seed. Ultra-high performance liquid chromatography equipped with quadrupole time-of-flight mass spectrometry(UHPLC-QTOF-MS) was applied for chemical profiling. Ultra-high performance liquid coupled with triple quadrupole mass spectrometry(UHPLC-Qq Q-MS) was employed to quantify AA-I and AA-II in different parts. It was found that the chemical compositions of the four parts varied both qualitatively and quantitatively. A total of 10 AAAs, including 5 aristolochic acids and 5 aristolactams, together with 3 alkaloids, were unambiguously or tentatively identified by UHPLC-QTOF-MS. The quantitatively analytical results obtained by UHPLC-Qq Q-MS showed that AA-I and AA-II exclusively accumulate in the seeds of A. contorta. These findings provide supporting data for the rational selection of medicinal parts.

关键词： Aristolochia contorta Aristolochic acids Ultra-high performance liquid chromatography quadrupole time-of-flight mass spectrometry triple quadrupole mass spectrometry Tissue-specific profiling

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