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.

开发了 PRiME（工艺、稳健性、改进、基质效应、易用性）传递净化程序，用于提取和纯化水飞蓟素 A 和 B、水飞蓟宾 A 和 B、异水飞蓟宾 A 和 B 以及水飞蓟宁。优化提取溶剂类型和上样量后，将粗提物用95%乙腈稀释至3 mL，然后加载到PRiME小柱上。通过超高效液相色谱和串联质谱 (UPLC-MS/MS) 分析洗脱液。通过碰撞诱导解离 (CID)，所有目标分析物在m/z 481 处被去质子化为 [MH] ^- ，主要碎片离子为m/z 463 ([MH ₂ OH] ^- )、453 ([M- CO-H] ^- ）、355（[MC ₆ H ₆ O ₃ -H] ^- ）、301（[M ₃₅₅ -CO ₂ -H] ^- ）和179（[C ₁₀ H ₁₁ O ₃ ] ^- ）。随后，该方法在线性（R ² > 0.9990）、日内精密度（1.02%–3.79%）、日间精密度（1.59%–4.87%）、灵敏度（LOD ≤ 0.45 μg·kg ^{− 1}且 LOQ ≤ 1.50 μg·kg ⁻¹ )，回收率 (76.9–103.4%，RSD < 8.90%)。最后，所提出的方案成功应用于八批S. marianum样品。不同产地批次的七种活性化合物的总含量有所不同。