Zhejiang Province Key Laboratory of Anesthesiology, Department of Anesthesiology, The Second Affiliated Hospital and Yuying Children's Hospital of Wenzhou Medical University, Wenzhou, P. R. China.
Institute of Seafood, Zhejiang Gongshang University, Hangzhou, P. R. China.
Electrophoresis. 2020 Mar;41(5-6):379-385. doi: 10.1002/elps.201900401.
Justicia procumbens is a food and medicine homologous variety, popularly used for making vegetable soups. In this study, a novel mesoporous silica was synthesized and used as the sorbent of SPE for the purification of lignans from J. procumbens. A laboratory-made SPE cartridge was packed with 100 mg of mesoporous silica, which was washed with 10% methanol and eluted using 0.8 mL acetonitrile after sample loading. Afterward, the extract was analyzed by ultra-performance liquid chromatography (UPLC) and MS/MS. All the lignans were efficiently separated in 6 min with the noise level in the range of 50-150 cps. 6'-Hydroxy justicidin B, 6'-hydroxy justicidin A, justicidin B, chinensinaphthol methyl ether, justicidin C, and neojusticdin A were identified to be the dominant molecular species in J. procumbens with contents of 0.065-0.37 mg/g in three tested sample batches from different geographic origins. In conclusion, the proposed mesoporous silica based SPE UPLC-MS/MS method is efficient in linearity (R = 0.9989-0.9996), sensitivity (LOD ≤0.13 μg/kg and LOQ ≤0.42 μg/kg), precision (RSD ≤3.12 and RSD ≤4.56), and recovery (83.42-96.11%, RSD ≤2.88%).
垂序商陆是一种药食同源的品种，常被用来制作蔬菜汤。本研究合成了一种新型介孔硅材料，并将其用作 SPE 的吸附剂，用于从垂序商陆中纯化木脂素。实验室自制的 SPE 小柱填充 100mg 介孔硅，在样品加载后，先用 10%甲醇洗涤，再用 0.8ml 乙腈洗脱。然后，采用超高效液相色谱（UPLC）和 MS/MS 对提取物进行分析。所有木脂素在 6 分钟内得到有效分离，噪音水平在 50-150cps 范围内。鉴定出 6'-羟基千金藤啶碱 B、6'-羟基千金藤啶碱 A、千金藤啶碱 B、千金藤素甲醚、千金藤素 C 和新千金藤定 A 是垂序商陆中的主要分子种类，在来自不同地理来源的 3 批测试样品中，含量在 0.065-0.37mg/g 之间。总之，所提出的基于介孔硅的 SPE-UPLC-MS/MS 方法在线性（R=0.9989-0.9996）、灵敏度（LOD≤0.13μg/kg 和 LOQ≤0.42μg/kg）、精密度（RSD≤3.12 和 RSD≤4.56）和回收率（83.42-96.11%，RSD≤2.88%）方面均表现良好。
