A new hybrid of silica aerogel with a Preyssler‐type polyoxometalate and MIL‐101(Cr) metal–organic framework was prepared and used as a highly porous fiber coating for headspace solid-phase microextraction of Ferulago angulata volatile components. Applying a permanent magnetic field to the sorbent increased the extraction efficiency for most of the plant’s components, up to 5.53 times. Optimization of the extraction parameters was carried out using a GC–MS instrument and by a simplex method. The extraction efficiency of the P5W30/MIL-101(Cr)/silica aerogel fiber exceeded 3.5 times of a mesoporous SBA-15 fiber. The prepared fiber was stable in multiple injections with relative standard deviations of 5.3 to 10.9% for 5 replicates. The proposed method was successfully applied to the extraction and identification of volatile components of some F. angulata samples. According to the results obtained by GC-FID, β-bourbonene, β-gurjunene, β-elemene and cedrenol were the main components of the plant.

制备了一种新型二氧化硅气凝胶与 Preyssler 型多金属氧酸盐和 MIL-101(Cr) 金属-有机骨架的混合物，并将其用作高度多孔的纤维涂层，用于顶空固相微萃取角豆挥发性成分。对吸附剂施加永久磁场可将植物大部分成分的提取效率提高至 5.53 倍。提取参数的优化使用 GC-MS 仪器和单一方法进行。P5W30/MIL-101(Cr)/二氧化硅气凝胶纤维的提取效率超过了介孔SBA-15纤维的3.5倍。制备的纤维在多次进样中稳定，5 次重复的相对标准偏差为 5.3% 至 10.9%。所提出的方法已成功应用于部分角鲽样品挥发性成分的提取和鉴定。根据 GC-FID 得到的结果，β-波旁烯、β- gurjunene、β-榄香烯和雪松酚是该植物的主要成分。