PRiME pass-through purification of lignans in Silybum marianum and UPLC-MS/MS analysis

Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences
Manman ZhangHaixing Wang

Abstract

A PRiME (process, robustness, improvements, matrix effects, ease of use) pass-through cleanup procedure was developed for the extraction and purification of silychristins A and B, silybins A and B, isosilybins A and B, and silydianin in Silybum marianum. After optimizing the extracting solvent types and the sample loading volume, the crude extract was diluted to 3 mL with 95% acetonitrile and then loaded on the PRiME cartridge. The eluate was analyzed by ultra-performance liquid chromatography and tandem mass spectrometry (UPLC-MS/MS). All the target analytes were deprotonated as [M-H]- at m/z 481 by conducting collision-induced dissociation (CID), and the major fragment ions were m/z 463 ([M-H2O-H]-), 453 ([M-CO-H]-), 355 ([M-C6H6O3-H]-), 301 ([M355-CO2-H]-), and 179 ([C10H11O3]-). Afterwards, this method was validated in terms of linearity (R2 > 0.9990), intra-day precision (1.02%-3.79%), inter-day precision (1.59%-4.87%), sensitivity (LOD ≤ 0.45 μg·kg-1 and LOQ ≤ 1.50 μg·kg-1), and recovery (76.9-103.4%, RSD < 8.90%). Finally, the proposed protocol was successfully applied to eight batches of S. marianum samples. The total content of the seven active compounds varied amongst the batches from different places of origin.

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