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液相色谱-质谱法同时测定蜂蜜中的吡咯里西啶生物碱和托烷生物碱

Simultaneous Determination of Pyrrolizidine and Tropane Alkaloids in Honey by Liquid Chromatography-mass Spectrometry.

作者信息

Kowalczyk Ewelina, Kwiatek Krzysztof

机构信息

Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, 24-100 Puławy, Poland.

出版信息

J Vet Res. 2022 Jul 5;66(2):235-243. doi: 10.2478/jvetres-2022-0032. eCollection 2022 Jun.

Abstract

INTRODUCTION

Pyrrolizidine alkaloids (PAs) and tropane alkaloids (TAs) are natural contaminants of honey and respectively hepatoxic and neurotoxic compounds. Because honey is a popular constituent of the human diet, it is relevant to warrant the safety of the product. For that reason, a method for simultaneous determination of PAs and TAs in honey based on liquid chromatography- mass spectrometry was developed.

MATERIAL AND METHODS

The analytical protocol used sulphuric acid extraction and solid-phase extraction purification. The developed procedure was subjected to validation in terms of linearity, selectivity, repeatability, reproducibility, limits of quantification and determination, matrix effect and uncertainty. A total of 29 honey samples were analysed for the determination of PAs and TAs.

RESULTS

All the evaluated validation parameters fulfilled the requirements of European Commission Decision 2002/657/EC. At least one of the monitored alkaloids was determined in 52% of the samples. Among the most abundant alkaloids were echimidine, intermedine and lycopsamine. The total PA concentrations ranged from 2.2 to 147.0 μg kg. Contrastingly, none of the monitored TAs was detected in the analysed samples. An assessment of the dietary exposure to PAs from the consumption of the contaminated honeys showed that three of them would pose a risk to consumers, especially if they were children.

CONCLUSION

A sensitive method suitable for simultaneous determination of PAs and TAs in honey was developed and validated. The analysis of 29 honey samples for PAs and TAs revealed that honey destined for retail could pose a risk to consumers.

摘要

引言

吡咯里西啶生物碱(PAs)和托烷生物碱(TAs)是蜂蜜中的天然污染物,分别为肝毒性和神经毒性化合物。由于蜂蜜是人类饮食中常见的成分,保证该产品的安全性很重要。因此,开发了一种基于液相色谱 - 质谱联用同时测定蜂蜜中PAs和TAs的方法。

材料与方法

分析方案采用硫酸萃取和固相萃取净化。所开发的方法在线性、选择性、重复性、再现性、定量和测定限、基质效应和不确定度方面进行了验证。共分析了29个蜂蜜样品以测定PAs和TAs。

结果

所有评估的验证参数均符合欧盟委员会第2002/657/EC号决定的要求。在52%的样品中测定出至少一种监测到的生物碱。含量最高的生物碱包括全缘千里光碱、间千里光碱和石蒜碱。PAs的总浓度范围为2.2至147.0μg/kg。相比之下,在所分析的样品中未检测到任何监测的TAs。对食用受污染蜂蜜导致的PAs膳食暴露评估表明,其中三种蜂蜜会对消费者构成风险,尤其是儿童。

结论

开发并验证了一种适用于同时测定蜂蜜中PAs和TAs的灵敏方法。对29个蜂蜜样品进行的PAs和TAs分析表明,零售蜂蜜可能对消费者构成风险。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/8fed/9281522/2781fa841371/jvetres-66-235-g001.jpg

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