金花茶中黄酮类活性成分的GC-MS分析

Application of GC-MS Technique to Analyze Active Ingredients of Flavonoids in Camellia chrysantha Flos

目的：建立石墨烯-搅拌棒吸附萃取（SBSE）结合气相色谱-质谱联用（GC-MS）分析金花茶中黄酮类活性成分并对总黄酮的相对含量进行测定。方法：自制稻草源活性炭制备石墨烯聚合物,实验中对影响SBSE的因素（萃取涂层选择、萃取温度和时间等）进行了优化,用GC-MS鉴定金花茶中黄酮类活性成分,在所得优化条件下采用峰面积归一化法对金花茶中总黄酮相对含量进行测定。结果：样品中黄酮类活性成分经鉴定有儿茶素,表没食子儿茶素（EGC）,儿茶酚（C）,槲皮素-7-O-葡萄糖苷,芦丁,异槲皮苷,花青素,槲皮素,山柰酚,儿茶素没食子酸酯（CG）,儿茶素没食子酸酯（CG）等,经检测金花茶中总黄酮相对含量（主要为槲皮素和山柰酚）达到3.0%。同一样品经6次测定,以金花茶总黄酮的总峰面积值为考察指标,其RSD 1.0%。结论：建立的SBSE-GC-MS方法分离鉴定出24个成分,测定金花茶总黄酮相对含量重复性较好,适于金花茶黄酮类成分的分析检测,为金花茶黄酮类活性成分的进一步研究提供了理论参考。

Objective： To establish a analytical method combining graphene-stir bar sorptive extraction（ SBSE） and chromatography-mass spectrometry（ GC-MS） for the active components of flavonoids in Camellia chrysantha flos and the relative content of total flavonoids. Method： Activated carbon from rice straw was made to prepare the graphene polymer,and the factors affecting SBSE（ such as selection of extraction coatings,extraction temperature and time） were optimized. Then GC-MS was used to identify the active components of flavonoids in C. chrysantha flos and determine the relative content of total flavonoids by using peak area normalization method under the optimized conditions. Result： Flavonoids in C. chrysantha flos were identified as catechin,epigallocatechin（ EGC）,catechol（ C）,quercetin-7-O-glucoside,rutin,isoquercitrin,quercetin,kaempferol,anthocyanins,epigallocatechin gallate（ CG）,and epigallocatechin gallate（ CG） etc. The relative content of total flavonoids（ mainly including quercetin and kaempferol） reached 3. 0%. After 6 tests of the same sample,the total peak area of the total flavonoids in C. chrysantha flos was used as the evaluation index,with a relative standard deviation（ RSD） of 1. 0%. Conclusion： The method separated and identified 24 components by SBSE-GC-MS,and the results indicated good reproducibility and appropriateness of the method to test the flavonoids in C. chrysantha flos,providing theoretical reference for further studies on flavonoids in C. chrysantha flos.