食品科学 ›› 2018, Vol. 39 ›› Issue (4): 176-187.doi: 10.7506/spkx1002-6630-201804027

• 成分分析 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时测定5 个产地花椰菜和西兰花中的23 种酚酸类化合物

马帅,王纪华,高媛,王蒙*,冯晓元*   

  1. (北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室(北京),农产品产地环境监测北京市重点实验室,北京 100097)
  • 出版日期:2018-02-25 发布日期:2018-02-02
  • 基金资助:
    国家农产品质量安全风险评估重大专项(GJFP201601503);公益性行业(农业)科研专项(201303075); 农业部农产品质量安全风险评估实验室(北京)开放课题(kfkt201701)

Simultaneous Determination of Twenty-Three Phenolic Acids in Cauliflower (Brassica oleracea L. var. botrytis L.) and Broccoli (B. oleracea?L. var. italica) from Five Producing?Places by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

MA Shuai, WANG Jihua, GAO Yuan, WANG Meng*, FENG Xiaoyuan*   

  1. (Beijing Research Center for Agricultural Standards and Testing, Risk Assessment Lab for Agro-Products (Beijing), Ministry of Agriculture, Beijing Municipal Key Laboratory of Agriculture Environment Monitoring, Beijing 100097, China)
  • Online:2018-02-25 Published:2018-02-02

摘要: 建立超高效液相色谱-串联质谱同时测定花椰菜和西兰花样品中23种酚酸类化合物的方法。采用Waters Acquity UPLC HSS T3色谱柱(2.1mm×150mm,1.8μm)分离,流动相为0.1%甲酸溶液(A)和0.1%甲酸-乙腈溶液(B),梯度洗脱流速为0.3mL/min,柱温为45℃,选择电喷雾离子源,多反应监测负离子模式进行扫描分析。23种酚酸类化合物在1.0~500.0μg/L范围内呈现良好的线性关系,相关系数(r2)均不低于0.992;方法精密度、重复性和稳定性良好,相对标准偏差均小于5.10%;加标回收率为81.32%~100.39%,相对标准偏差均不大于6.21%。采用所建立的方法对5个产地的花椰菜和西兰花中的酚酸类化合物进行测定。该方法分析时间短、灵敏度高且重复性好,适用于花椰菜、西兰花及其他果蔬中酚酸类化合物的同时测定。

关键词: 超高效液相色谱-串联质谱, 酚酸, 花椰菜, 西兰花

Abstract: A method for the simultaneous determination of twenty-three phenolic acids in cauliflower (Brassica oleracea L. var. botrytis L.) and broccoli (B. oleracea L. var. italica) was developed by ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target analytes were separated on an Acquity UPLC HSS T3 column (2.1 mm × 150 mm, 1.8 μm) under a gradient elution mode using a mobile phase consisting of 0.1% formic acid and 0.1% formic acid acetonitrile. The flow rate was 0.3 mL/min and the column temperature was 45 ℃. The target compounds were analyzed in the negative ion multiple reaction monitoring (MRM) mode. Good linear relationships were obtained for all the analytes in the concentration range of 1.0–500.0 μg/L were obtained with high correlation coefficients over 0.992. The precision, repeatability and stability, expressed as relative standard deviation (RSD), were lower than 5.10%. The recoveries from spiked samples ranged from 81.32% to 100.39%, with RSD below 6.21%. The proposed method was applied to the determination of phenolic compounds in broccoli and cauliflower samples collected from five different cities. The method showed time saving, high sensitivity, and good repeatability, and was suitable for the simultaneous determination of phenolic compounds in cauliflower, broccoli and other vegetables.

Key words: UPLC-MS/MS, phenolic acids, cauliflower (Brassica oleracea L. var. botrytis L.), broccoli (B. oleracea L. var. italica)

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