An Ultra-High Performance Liquid Chromatography-Mass Spectrometry Method Based on Solid Phase Extraction Was Developed for the Analysis of Polyphenols in Prunus Mume Sieb. et Zucc.

Weiting Wang, Xuanxuan Fan, Naidong Chen, Jingwen Hao, Manman Zhang, Zhengjun Xie
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Abstract

Background: Prunus mume Sieb. et Zucc. (P. mume) is rich in various phenolic compounds; however, there is a lack of effective quality evaluation methods.

Objective: The aim of this study was to establish and validate a quality evaluation method that combines composition and activity to evaluate P. mume.

Method: Phenolic compounds were quantified using an ultra-high performance liquid chromatography-diode array detector (UPLC-DAD) and identified using quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS). Solid-phase extraction (SPE) method was used for enrichment and purification. Chromatographic column: Eclipse Plus-C18 (2.1 × 50 mm, 5 μm); column temperature: 30 °C; detection wavelength: 325 nm, flow rate: 0.25 mL/min. 2,2'-azinobis- 3-ethylbenzthiazoline-6-sulphonate (ABTS) and ferric ion-reducing antioxidant power (FRAP) assays were used to determine the antioxidant activity of P. mume. In addition, tyrosinase inhibitory activity (TIA) was verified for the first time.

Results: Twelve major phenolic compounds were identified, among which taxifolin and ferulic acid were first detected in P. mume. The established UPLC-DAD method exhibited a strong linear relationship (R2 = 0.9999). The LOD and LOQ of the standard compounds were in the ranges of 0.001-0.014 ng/g and 0.009-0.048 ng/g, respectively. The method exhibited good linearity, precision, stability and repeatability. The phenolic compound content was in the range of 0.38-75.88 mg/g. In addition, P. mume extract showed excellent ABTS•+ radical scavenging capacity (IC50 = 108.93 ± 9.43 μg/mL), FRAP (10.23 ± 0.11 μM), and TIA (IC50 = 4.79 ± 0.08 mg/mL).

Conclusions: The established quality control method based on composition and activity is dependable and can be used for the quality control of P. mume.

Highlights: SPE chromatographic analysis method is reliable and can provide a reference for quality control methods for the combination of ingredients and activity in flower-based foods.

背景:梅(Prunus mume Sieb:梅(Prunus mume Sieb. et Zucc.)富含多种酚类化合物,但缺乏有效的质量评价方法:本研究旨在建立和验证一种结合成分和活性的质量评价方法,以评价梅花:方法:使用超高效液相色谱-二极管阵列检测器(UPLC-DAD)对酚类化合物进行定量,并使用四极杆飞行时间质谱(UPLC-Q-TOF-MS)进行鉴定。固相萃取(SPE)法用于富集和纯化。色谱柱:Eclipse Plus-C18 (2.1 × 50 mm, 5 μm);柱温:30 °C;检测波长:5 μm:检测波长:325 nm,流速:0.25 mL/min:0.25 mL/min。采用 2,2'-azinobis- 3-ethylbenzthiazoline-6-sulphonate (ABTS) 和铁离子还原抗氧化力 (FRAP) 法测定 P. mume 的抗氧化活性。此外,还首次验证了酪氨酸酶抑制活性(TIA):结果:共鉴定出 12 种主要酚类化合物,其中 taxifolin 和阿魏酸是首次在梅花中检测到。所建立的 UPLC-DAD 方法线性关系良好(R2 = 0.9999)。标准化合物的检出限(LOD)和定量限(LOQ)分别为0.001~0.014 ng/g和0.009~0.048 ng/g。该方法具有良好的线性、精密度、稳定性和重复性。酚类化合物的含量范围为 0.38-75.88 mg/g。此外,P. mume 提取物还表现出优异的 ABTS-+ 自由基清除能力(IC50 = 108.93 ± 9.43 μg/mL)、FRAP(10.23 ± 0.11 μM)和 TIA(IC50 = 4.79 ± 0.08 mg/mL):基于成分和活性建立的质量控制方法是可靠的,可用于 P. mume 的质量控制:SPE色谱分析方法可靠,可为花基食品中成分和活性组合的质量控制方法提供参考。
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