超高效液相色谱-串联质谱法测定甜樱桃果皮中花青苷类物质

Determination of anthocyanins in the peel of sweet cherry by ultra performance liquid chromatographytandem mass spectrometry

建立了甜樱桃果皮中7种花青苷类物质的超高效液相色谱-串联质谱（UPLC-MS/MS）定性和定量检测方法。样品经0.1%（v/v）盐酸甲醇提取液提取,AB-8型大孔吸附树脂净化,在电喷雾离子源正离子（ESI＋）多反应监测（MRM）模式下对目标物质进行定性和定量分析。结果表明：7种目标化合物的定量限为0.26-1.42μg/kg;在0-100μg/L范围内呈现很好的线性关系,相关系数（r2）为0.996 4-0.999 3;方法的加标回收率为97.2%-105.4%,相对标准偏差（RSD）为1.9%-5.8%。采用该方法对甜樱桃红色品种＂美早＂和黄色品种＂13-33＂成熟果实样品进行了分析,发现主要花青苷类物质的成分和含量存在显著性差异。该方法操作简单,灵敏度高,重复性好,花青苷类物质的分析覆盖面广,可用于甜樱桃中花青苷类成分快速鉴定及含量测定。

A method for the determination of seven anthocyanins in the peel of sweet cherry was developed by ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS/MS）. The sample was extracted by methanol containing 0. 1%（ v/v）hydrochloric acid,and then purified by AB-8 macroporous resins. The separation was carried out on a Phenomenex Ki-netex column（100 mm＆#215;4. 6 mm,2. 6 μm）with mobile phase of 0. 1%（v/v）formic acid aque-ous solution containing 5 mmol/L ammonium formate and methanol. The sample solution was detected by UPLC-MS/MS with ESI under positive ion and multi reaction monitoring（ MRM ） modes. The results showed that the limits of quantification（ LOQs）for the seven target com-pounds were 0. 26-1. 42 μg/kg. The seven anthocyanin standards showed a good linearity in the range of 0-100 μg/L with the correlation coefficients（r^2）of 0. 996 4-0. 999 3. The average recoveries of the seven anthocyanins were 97. 2%-105. 4%,and the relative standard deviations （ RSDs）were 1. 9%-5. 8%. The mature fruit samples of sweet cherry red variety“Tieton”and the yellow variety“13-33”were analyzed by this method. The results showed that the anthocya-nin composition and contents were significantly different between the two varieties. This meth-od can be used for rapid identification and the determination of anthocyanin components in sweet cherry fruits due to its simple operation,high sensitivity,good reproducibility and cover-ing a wide range of anthocyanins.