超高效液相色谱-离子淌度-四极杆飞行时间质谱法识别精河枸杞中多酚类化合物

Identification of polyphenols in Jinghe Lycium barbarum by ultra performance liquid chromatography-ion mobility-quadrupole time of flight-mass spectrometry

目的分析不同时期、不同品种新疆精河枸杞总酚和总黄酮含量差异,识别其多酚类化合物成分,并对主要成分进行定性定量分析。方法采集新疆精河县不同时期、不同品种枸杞果实样本139份,通过福林酚比色法、三氯化铝比色法测定枸杞提取物中总多酚、总黄酮含量,建立超高效液相色谱-离子淌度-四极杆飞行时间质谱法(ultra performance liquid chromatography-ion mobility-quadrupole time of flight-mass spectrometry,UPLC-IM-QTOF-MS)对枸杞提取物中多酚类化合物进行鉴定。结果2020年和2021年枸杞总酚、总黄酮含量分别为6.855~9.438、13.740~26.714mg/g和8.461~10.814、15.895~29.500mg/g;其中,总酚、总黄酮在秋果枸杞的含量均高于夏果枸杞,不同品种(宁杞七号、1801号、宁杞九号)枸杞多酚含量均存在显著性差异(P<0.05);初步筛选并识别出精河枸杞中含有28种(响应值>1000)多酚类物质,包括黄酮类18种、酚酸类8种、鞣酸类2种,主要多酚成分为:芦丁、异槲皮素、对-香豆酸、莰菲醇-3-O-芸香糖苷、异鼠李素、异鼠李素-3-O-芸香糖苷,含量分别为(116.23±30.31)、(84.34±12.05)、(14.73±4.06)、(19.27±6.38)、(5.42±1.41)、(4.50±1.08)μg/g。结论同一产区,不同时期、不同品种枸杞多酚含量存在显著性差异;精河枸杞中含有丰富的黄酮类和多酚类化合物,芦丁、对-香豆酸是现有识别多酚类成分中最主要的多酚类化合物。

Objective To analyze the content difference of total phenol and flavonoids in different varieties of Jinghe Lycium barbarum in different periods,identify the polyphenolic compounds,and qualitatively and quantitatively analyze the main components.Methods A total of 139 samples of Lycium barbarum fruits from different periods and varieties were collected from Jinghe County,Xinjiang,and the content of total phenols and total flavonoids in Lycium barbarum extract was determined by Folin colorimetric method and aluminum trichloride colorimetric method,and ultra performance liquid chromatography-ion mobility-quadrupole time of flight-mass spectrometry(UPLC-IM-QTOF-MS)was established to identify the polyphenolic compounds in Lycium barbarum extract.Results The content of total phenols and total flavonoids of Lycium barbarum in 2020 and 2021 were 6.855-9.438,13.740-26.714 mg/g and 8.461-10.814,15.895-29.500 mg/g,respectively.Among them,the content of total phenols and total flavonoids in autumn fruit Lycium barbarum was higher than that of summer fruit Lycium barbarum,and the polyphenol content of different varieties(Ningqi 7#,1801#,Ningqi 9#)of Lycium barbarum in different periods had significant differences(P<0.05).Twenty-eight kinds of polyphenols(response value>1000)were preliminary identified in Jinghe Lycium barbarum,including 18 kinds of flavonoids,8 kinds of phenolic acids,and 2kinds of tannic acid.The main polyphenol components were rutin,isoquercetin,p-coumaric acid,camphenol-3-O-rutin,isorhamnetin,isorhamnetin-3-O-rutin,with the content of(116.23±30.31),(84.34±12.05),(14.73±4.06),(19.27±6.38),(5.42±1.41)and(4.50±1.08)μg/g,respectively.Conclusion There are significant differences in polyphenol content of Lycium barbarum at different periods and varieties in the same production area.Jinghe Lycium barbarum is rich in flavonoids and polyphenols,among which rutin and p-coumaric acid are the most important polyphenols.