食品科学 ›› 2021, Vol. 42 ›› Issue (18): 185-190.doi: 10.7506/spkx1002-6630-20200915-188

• 成分分析 • 上一篇    下一篇

黑果枸杞化学成分的UPLC-Triple TOF/MS分析及其总花色苷类含量测定

甘小娜,王辉俊,李廷钊,李波   

  1. (1.安利(中国)研发中心,上海 201203;2.上海中医药大学中药研究所,上海 201203)
  • 发布日期:2021-09-29
  • 基金资助:
    上海市自然科学基金项目(20ZR1458100)

Lycium ruthenicum Murray Fruit: Chemical Composition Analysis by Ultra-high Performance Liquid Chromatography Coupled to Triple Time of Flight Mass Spectrometry and Determination of Total Anthocyanins

GAN Xiaona, WANG Huijun, LI Tingzhao, LI Bo   

  1. (1. Amway (China) R&D Center, Shanghai 201203, China; 2. Institute of Chinese Materia Medica, Shanghai University of traditional Chinese Medicine, Shanghai 201203, China)
  • Published:2021-09-29

摘要: 采用超高效液相色谱-飞行时间质谱联用技术对黑果枸杞中的化学成分进行分析,通过多级离子碎片信息,结合天然产物高分辨质谱数据库及相关文献进行推断;采用超高效液相色谱仪,使用Acquity UPLC BEH C18柱(2.1 mm×50 mm,1.7 μm),以0.1%三氟乙酸-10%甲酸溶液及甲酸-水-甲醇-乙腈(1∶5∶2∶2,V/V)为流动相进行梯度洗脱,检测波长530 nm,对黑果枸杞中的总花色苷进行定量分析;黑果枸杞中的总花色苷含量以矢车菊素-3-O-葡萄糖苷为标准计算。从黑果枸杞中共鉴定出化合物30 个,其中包括生物碱类化合物13 个、花色苷类化合物13 个。矢车菊素-3-O-葡萄糖苷在0.005~0.08 mg/mL质量浓度范围内线性关系良好(R=0.999 9);平均加样回收率为95.45%,相对标准偏差为2.62%。本方法可快速、高效地鉴定黑果枸杞中的化合物;花色苷含量测定方法重复性好、准确度高,有助于提高黑枸杞的品质控制。

关键词: 黑果枸杞;超高效液相色谱-飞行时间质谱;定性鉴别;总花色苷;含量测定

Abstract: A rapid and precise method to identify the phytochemicals in the fruit of Lycium ruthenicum Murray (LRM) was established using ultra-high performance liquid chromatography coupled to triple time of flight mass spectrometry (UPLC-Triple TOF/MS) with multistage fragment ions data, the natural compounds mass spectral database and related data reported in the literature. Total anthocyanins in LRM were quantitatively analyzed by UPLC equipped with an Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm). Gradient elution was carried out using 0.1% trifluoroacetic acid-10% formic acid aqueous solution as mobile phase A and formic acid:water:methanol:acetonitrile (1:5:2:2, V/V) as mobile phase B. The detection wavelength was 530 nm. The total content of anthocyanins was calculated as cyanidin-3-O-glucoside. Thirty compounds were identified from LRM, including 13 alkaloids and 13 anthocyanins. The concentration of cyanidin-3-O-glucoside in the range of 0.005–0.08 mg/mL had good linear relationship with the peak area (R = 0.999 9). The average recovery for spiked samples was 95.45%, with a relative standard deviation (RSD) of 2.62%. The chemical constituents of LRM were identified rapidly and efficiently by UPLC-Triple TOF/MS, and the UPLC method for the determination of total anthocyanins was highly repeatable and accurate and could be used for the quality evaluation and control of LRM.

Key words: Lycium ruthenicum Murry; ultra-high performance liquid chromatography coupled to triple time of flight mass spectrometry; identification; total anthocyanins; determination

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