{"title":"建立了一种基于固相萃取的超高效液相色谱-质谱法分析梅子中多酚类物质的方法。调查。","authors":"Weiting Wang, Xuanxuan Fan, Naidong Chen, Jingwen Hao, Manman Zhang, Zhengjun Xie","doi":"10.1093/jaoacint/qsaf028","DOIUrl":null,"url":null,"abstract":"<p><strong>Background: </strong>Prunus mume Sieb. et Zucc. (P. mume) is rich in various phenolic compounds; however, there is a lack of effective quality evaluation methods.</p><p><strong>Objective: </strong>The aim of this study was to establish and validate a quality evaluation method that combines composition and activity to evaluate P. mume.</p><p><strong>Methods: </strong>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). A solid-phase extraction (SPE) method was used for enrichment and purification. An Eclipse Plus-C18 (2.1 × 50 mm, 5 μm) column was used for separation at a flow rate of 0.25 mL/min, column temperature of 30°C, and detection wavelength of 325 nm. 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.</p><p><strong>Results: </strong>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 limit of detection and limit of quantitation 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 (half maximal inhibitory concentration (IC50) = 108.93 ± 9.43 μg/mL), FRAP (10.23 ± 0.11 μM), and TIA (IC50 = 4.79 ± 0.08 mg/mL).</p><p><strong>Conclusion: </strong>The established QC method based on composition and activity is dependable and can be used for QC of P. mume.</p><p><strong>Highlights: </strong>The chromatographic analysis method is reliable and can provide a reference for QC methods for the determination of ingredients and activity in flower-based foods.</p>","PeriodicalId":94064,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"637-647"},"PeriodicalIF":0.0000,"publicationDate":"2025-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"An Ultra-High Performance Liquid Chromatography-Mass Spectrometry Method Based on Solid-Phase Extraction Developed for the Analysis of Polyphenols in Prunus Mume Sieb. et Zucc.\",\"authors\":\"Weiting Wang, Xuanxuan Fan, Naidong Chen, Jingwen Hao, Manman Zhang, Zhengjun Xie\",\"doi\":\"10.1093/jaoacint/qsaf028\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><strong>Background: </strong>Prunus mume Sieb. et Zucc. (P. mume) is rich in various phenolic compounds; however, there is a lack of effective quality evaluation methods.</p><p><strong>Objective: </strong>The aim of this study was to establish and validate a quality evaluation method that combines composition and activity to evaluate P. mume.</p><p><strong>Methods: </strong>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). A solid-phase extraction (SPE) method was used for enrichment and purification. An Eclipse Plus-C18 (2.1 × 50 mm, 5 μm) column was used for separation at a flow rate of 0.25 mL/min, column temperature of 30°C, and detection wavelength of 325 nm. 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.</p><p><strong>Results: </strong>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 limit of detection and limit of quantitation 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 (half maximal inhibitory concentration (IC50) = 108.93 ± 9.43 μg/mL), FRAP (10.23 ± 0.11 μM), and TIA (IC50 = 4.79 ± 0.08 mg/mL).</p><p><strong>Conclusion: </strong>The established QC method based on composition and activity is dependable and can be used for QC of P. mume.</p><p><strong>Highlights: </strong>The chromatographic analysis method is reliable and can provide a reference for QC methods for the determination of ingredients and activity in flower-based foods.</p>\",\"PeriodicalId\":94064,\"journal\":{\"name\":\"Journal of AOAC International\",\"volume\":\" \",\"pages\":\"637-647\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2025-07-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of AOAC International\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.1093/jaoacint/qsaf028\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of AOAC International","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.1093/jaoacint/qsaf028","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
An Ultra-High Performance Liquid Chromatography-Mass Spectrometry Method Based on Solid-Phase Extraction Developed for the Analysis of Polyphenols in Prunus Mume Sieb. et Zucc.
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.
Methods: 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). A solid-phase extraction (SPE) method was used for enrichment and purification. An Eclipse Plus-C18 (2.1 × 50 mm, 5 μm) column was used for separation at a flow rate of 0.25 mL/min, column temperature of 30°C, and detection wavelength of 325 nm. 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 limit of detection and limit of quantitation 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 (half maximal inhibitory concentration (IC50) = 108.93 ± 9.43 μg/mL), FRAP (10.23 ± 0.11 μM), and TIA (IC50 = 4.79 ± 0.08 mg/mL).
Conclusion: The established QC method based on composition and activity is dependable and can be used for QC of P. mume.
Highlights: The chromatographic analysis method is reliable and can provide a reference for QC methods for the determination of ingredients and activity in flower-based foods.