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Updated: Feb 8, 2026

Solid-phase Synthesis of [4.4] Spirocyclic Oximes

Solid-phase Synthesis of [4.4] Spirocyclic Oximes

Published on: February 6, 2019

ゴマ油中の13の複素環式アミンを高感度にUPLC-MS/MSで定量するための、処理済み松花粉に基づく分散固相抽出法の開発

Baocheng Ji¹, Yanxin Wang², Li Ma²

¹College of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou, China; Key Laboratory of Cold Chain Food Processing and Safety Control (Zhengzhou University of Light Industry), Ministry of Education, Zhengzhou, China; Henan Key Laboratory of Cold Chain Food Quality and Safety Control, Zhengzhou University of Light Industry, Zhengzhou, China; Henan Province Engineering Research Center of Meat Precision Processing and Quality Safety Control, Zhengzhou, China.

Journal of chromatography. A

|February 6, 2026

Abstract:

A rapid, convenient, and efficient dispersive solid-phase extraction approach, integrating ultraperformance liquid chromatography-tandem mass spectrometry and pretreated pine pollen, was developed for sensitive quantification of 13 heterocyclic amines (HCAs) in sesame oil. Critical parameters, namely sorbent type and dosage, adsorption mode and duration, detergent dosage, eluent additive and volume, and elution cycles, were systematically optimized to evaluate their effects on the HCA recovery. The proposed method was verified for all the 13 HCAs, demonstrating favorable analytical characteristics with remarkable linear relationships (coefficient of determination, R² ≥ 0.998), adequate recoveries (64.2%-99.4%), acceptable intra- and inter-day precision (relative standard deviations ≤ 10.4%), and low limits of detection (0.02-0.83 μg/kg) and quantification (0.07-2.70 μg/kg). The proposed approach offers distinct advantages, including rapidity, simplicity, cost-effectiveness, and minimized organic solvent consumption, demonstrating great potential for accurately analyzing HCAs in complex food matrices.

キーワード:

食用油複素環式アミン LC-MS 松花粉 d-SPE

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