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通过高效液相色谱-电喷雾串联质谱和核磁共振技术对竹笋中 p-苯氧苯甲醛的鉴定和结构解析。

Identification and structure elucidation of a p-phenoxybenzaldehyde in bamboo shoots by HPLC-ESI/MS/MS and NMR.

机构信息

Gyeong-In Regional Korea Food and Drug Administration, Juan-Dong 120, Nam-Gu, Incheon 402-835, Korea.

出版信息

J Agric Food Chem. 2011 Nov 9;59(21):11579-84. doi: 10.1021/jf2025727. Epub 2011 Oct 14.

DOI:10.1021/jf2025727
PMID:21981589
Abstract

In this study, a derivative of p-phenoxybenzaldehyde in bamboo shoots was investigated. Bamboo shoots were ground and extracted with water, and an aqueous suspension was purified by SPE using Oasis HLB cartridges. After the SPE procedure, the analytes were analyzed by HPLC with refractive index detection (HPLC-RI). In the HPLC-RI analysis for sucralose, a putative sucralose was detected. In the subsequent HPLC-PDA analysis, the suspicious peak showed a unique UV absorption spectrum with the maximum wavelength at 285 nm indicating the existence of an aromatic ring. The contents of the unknown compound in bamboo shoot products ranged from 0.01 to 0.15 mg/g. The identity of the unknown compound was further confirmed by HPLC-ESI/MS/MS. The molecular weight of the unknown compound was determined to be 244. The chemical structure of the unknown compound was elucidated on the basis of NMR spectroscopic analyses ((1)H, (13)C, DEPT, COSY, HMQC, and HMBC). Finally, the structure of the unknown compound was characterized as 4-(4-dihydroxymethylphenoxy)benzaldehyde.

摘要

在这项研究中,研究了竹笋中对苯氧基苯甲醛的衍生物。将竹笋研磨并用水提取,然后通过 SPE 使用 Oasis HLB 小柱对水悬浮液进行纯化。SPE 后,通过 HPLC-RI 分析进行分析。在 HPLC-RI 分析中,检测到了一种假定的三氯蔗糖。在随后的 HPLC-PDA 分析中,可疑峰显示出独特的紫外吸收光谱,最大波长在 285nm 处,表明存在芳环。竹笋产品中未知化合物的含量在 0.01 至 0.15mg/g 之间。通过 HPLC-ESI/MS/MS 进一步确认了未知化合物的身份。未知化合物的分子量确定为 244。根据 NMR 谱分析(1H、13C、DEPT、COSY、HMQC 和 HMBC)阐明了未知化合物的化学结构。最后,将未知化合物的结构表征为 4-(4-二羟甲基苯氧基)苯甲醛。

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