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采用高效液相色谱-荧光检测法,通过柱前衍生化同时测定中药中 6 种α-二羰基化合物。

Simultaneous determination of six α-dicarbonyl compounds in traditional Chinese medicines using high-performance liquid chromatography-fluorescence detector with pre-column derivatization.

机构信息

School of Pharmacy, Binzhou Medical University, Yantai, P. R. China.

出版信息

J Sep Sci. 2023 Oct;46(19):e2300435. doi: 10.1002/jssc.202300435. Epub 2023 Aug 7.

DOI:10.1002/jssc.202300435
PMID:37548124
Abstract

A reliable method for determination of six α-dicarbonyl compounds in traditional Chinese medicines was first developed and validated by high-performance liquid chromatography-fluorescence detector with pre-column derivatization. α-Dicarbonyl compounds in traditional Chinese medicines were extracted and derivatized with 2,3-diaminaphthalene. The derivatization procedure of six α-dicarbonyl compounds was confirmed by high-resolution mass spectrometry. The limits of quantitation for six α-dicarbonyl compounds ranged from 3.70 × 10 to 2.21 × 10  μM. The established method showed good linearity (regression coefficient > 0.9990), precision (relative standard deviation < 3.37%), and high recovery (97.8%∼113.1%). The developed method was successfully applied to detect the six α-dicarbonyl compounds in traditional Chinese medicines. The result exhibited six α-dicarbonyl compounds was found in the 15 kinds of traditional Chinese medicines, which suggested us that the determination of α-dicarbonyl compounds should be paid more attention in the quality control of traditional Chinese medicines.

摘要

首次建立并验证了高效液相色谱-荧光检测法(HPLC-FLD)用于测定中药材中 6 种α-二羰基化合物。采用 2,3-二氨基萘(2,3-DN)对中药材中的α-二羰基化合物进行提取和衍生化。通过高分辨质谱(HRMS)确认了 6 种α-二羰基化合物的衍生化过程。6 种α-二羰基化合物的定量限(LOQ)范围为 3.70×10~2.21×10 μM。该方法具有良好的线性(相关系数>0.9990)、精密度(相对标准偏差<3.37%)和高回收率(97.8%∼113.1%)。该方法成功应用于检测中药材中的 6 种α-二羰基化合物。结果表明,在 15 种中药材中均发现了 6 种α-二羰基化合物,这提示我们在中药材质量控制中应更加关注α-二羰基化合物的测定。

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