许亦峰

摘 要：利用QuEChERS結合UPLC-MS/MS建立叶用甘薯中黄酮类物质的提取检测方法。以福菜薯18为材料，选定芦丁等7种黄酮类物质，试验确定流动相、质谱条件、净化剂等条件，从而确定叶用甘薯中黄酮类物质的提取检测方法。结果表明：以0.2 g C18作为净化剂，流动相（A）0.1%甲酸水-（B）乙腈，芦丁、异槲皮苷、二氢槲皮素、斛皮苷、槲皮素、柚皮素、山奈酚等7种黄酮类物质的碰撞能分别为-23/-40、44/27、23/32、27/42、-31/-29、25/24、-33/-31，7种黄酮类物质在5 min内完全分离，在0.05～1 μg·mL-1范围内线性良好（R2>0.99），芦丁、异槲皮苷、二氢槲皮素、斛皮苷、槲皮素、柚皮素、山奈酚等7种黄酮类物质回收率依次为96.52%～97.64%、97.26%～98.74%、92.95%～94.62%、96.23%～97.65%、90.23%～92.56%、99.12%～101.56%、83.65%～84.64%。基质效应分析中芦丁、异槲皮素ME在100%～120%，表现为弱的基质增强效应，可以忽略;槲皮素、山奈酚ME在120%～150%，表现为中等基质增强效应;二氢槲皮素ME大于150%，表现为强基质增强效应;槲皮苷、柚皮素ME均小于50%，表现为强基质抑制效应。对福菜薯18中7种黄酮类物质检测发现，福菜薯18中不含有二氢槲皮素，异槲皮素含量最高、其次为芦丁。该方法专一性强、灵敏度高、重复性好，为叶用甘薯中黄酮类物质的提取检测提供参考依据。

关键词：QuEChERS法;液质联用色谱仪;叶用甘薯;黄酮化合物

中图分类号：S 531   文献标志码：A   文章编号：0253-2301（2021）11-0055-08

DOI： 10.13651/j.cnki.fjnykj.2021.11.009

Determination of Seven Flavonoids in the Leaf-used Sweet Potatoes byMeans of QuEChERS Combined with UPLC-MS/MS

XU Yi-feng

（Ningde Inspection and Testing Center for Agricultural Product Quality andSafety， Ningde， Fujian 352100， China）

Abstract： The extraction and detection method of flavonoids in the leaf-used sweet potatoes was established by using the QuEChERS combined with UPLC MS/MS. By taking Fucaishu 18 as the material， and selecting the seven flavonoids including rutinum， isoquercitrin， taxifolin， quercitrin， quercetin， naringenin and kaempferol， the conditions such as the flow phase， mass spectrometry conditions， and purifying agent were determined in the experiment， so as to determine the extraction and detection method of flavonoids in the leaf-used sweet potatoes. The results showed that with 0.2 g C18 as the purifying agent and 0.1 % formic acid water （A）- acetonitrile （B） as the flow phase， the collision energies of rutinum， isoquercitrin， taxifolin， quercitrin， quercetin， naringenin and kaempferol were -23/-40， 44/27， 23/32， 27/42， -31/-29， 25/24 and -33/-31， respectively. The seven flavonoids were completely separated within 5 min with good linearity in the range of 0.05-1 μg·mL-1 （R2 > 0.99）. The recoveries of rutinum， isoquercitrin， taxifolin， quercitrin， quercetin， naringenin and kaempferol were 96.52%-97.64%， 97.26%-98.74%， 92.95%-94.62%， 96.23%-97.65%， 90.23%-92.56%， 99.12%-101.56%， and 83.65%-84.64%， respectively. In the matrix effect analysis， rutinum and isoquercitrin ME ranged from 100% to 120%， which showed the weak matrix enhancing effect and could be ignored. Quercetin and kaempferol ME ranged from 120% to 150%， showing the moderate matrix enhancing effect. Taxifolin ME was more than 150%， showing the strong matrix enhancing effect， while quercitrin and naringenin ME were both lower than 50%， showing the strong matrix inhibition effect. The seven flavonoids in Fucaishu 18 were detected， and it was found that Fucaishu 18 did not contain taxifolin， and the content of isoquercitrin in it was the highest， followed by rutinum. The method had strong specificity， high sensitivity and good reproducibility， which could provide reference for the extraction and detection of flavonoids in the leaf-used sweet potatoes.

Key words： QuEChERS method; Liquid chromatography-mass spectrometry; Leaf-used sweet potatoes; Flavonoids

叶用甘薯，俗称地瓜叶、番薯叶，属旋花科牵牛花属草本匍匐性蔓生植物，是经人工选择性培育出的专门供人们食用幼嫩茎叶的甘薯品种[1]。叶用甘薯营养丰富，与白菜、菠菜、韭菜、芹菜、茄子、胡萝卜、番茄、甘蓝等13种蔬菜相比，其所含的蛋白质、纤维素、胡萝卜素、烟酸、脂肪、碳水化合物、钙、磷、铁等13项营养成分均居首位[2]。除此……