基于质谱裂解规律和UPLC-Q-TOF技术的玛咖酰胺类化合物筛查检测

Research on Screening and Detection Technology of Macamides with Mass Fragmentation Patterns and UPLC-Q-TOF

摘要:

本研究基于电荷或游离基中心诱导理论归纳了典型苄基和间甲氧基苄基玛咖酰胺类化合物的UPLC-Q-TOF质谱裂解规律，搭建了定性筛查谱库，同时建立了4种玛咖酰胺的定量检测技术。谱库包括保留时间、准分子离子及碎片离子的质荷比和分子结构等相关信息。结果表明，玛咖酰胺类化合物(A-J)可充分分离，出峰时间依次为5.83、5.32、5.93、6.50、6.40、5.23、7.32、6.58、6.47、7.32 min，利用谱库筛查时10种玛咖酰胺均可匹配10个以上碎片信息且质量分析误差在10 Mu以内；定量检测时4种玛咖酰胺（Mb18:3、Mo18:2、Mb18:2、Mb16）的检出限分别为0.50、1.20、1.20、0.50 mg/kg，定量限分别为1.50、3.60、3.60、1.50 mg/kg，平均回收率在81.64%~113.00%，且RSD均小于10%。本方法具有高准确性和精密度，对于玛咖及其制品的产地溯源、真假鉴别、质量分级和市场监管具有重要意义。

Abstract:

A qualitative screening library from the mass fragmentation patterns of benzyl and m-methoxybenzyl macamides was constructed based on the theory of charge or free radical center induction by ultra performance liquid chromatography-quadrupole-time of flight(UPLC-Q-TOF), and a quantitative determination method for 4 macamides was also established. The library includes retention time, mass-to-charge ratio and molecular structure of the excimer ions and fragment ions, and other information. The results showed that not only ten macamides were completely separated, but also more than 10 fragment ions for each macamide could be matched in library with a mass analysis error smaller than 10 Mu. The peak times of the macaamides (A-J) were 5.83, 5.32, 5.93, 6.50, 6.40, 5.23, 7.32, 6.58, 6.47, 7.32 min, respectively. In quantitative detection, the detection limits of 4 macamides (Mb18:3, Mo18:2, Mb18:2, Mb16) were 0.50, 1.20, 1.20, 0.50 mg/kg, respectively, and the quantitative limits were 1.50, 3.60, 3.60, 1.50 mg/kg, respectively. An average recovery rate ranged from 81.6% to 113.0% (RSD<10%) for 4 macamides. This method had high accuracy and precision, puting great significance for origin traceability, identification, quality classification and market supervision of maca and its products.