MilliporeSigma, 811 Paloma Drive Suite A, Round Rock, TX 78665-2402, United States.
U.S. Department of Health and Human Services, National Institutes of Health, Office of Dietary Supplements, 6705 Rockledge Drive, Bethesda, MD 20817, United States.
J AOAC Int. 2024 Jul 4;107(4):663-678. doi: 10.1093/jaoacint/qsae025.
Dietary supplements derived from botanicals are commonly consumed and investigated in biomedical studies for their potential health benefits. Accurate identification and quantification of key chemical constituents from botanical ingredients is necessary for consistent product preparations and reproducible research results. Manufacturers need quantitative reference materials of the chemical constituents of interest to verify the content of ingredients and products. The rigor and reproducibility of biomedical research is enhanced through thorough characterization of the interventions used in mechanistic, clinical, and safety investigations. Quantitative reference materials enable reliable product quality assessments and reproducible research results.
Solution-based certified reference material (CRM) mixes were developed as calibrants for phytochemicals in ginger and kava. The kava CRM contained yangonin, desmethoxyyangonin, dihydrokavain, DL-kavain, methysticin, dihydromethysticin, flavokawain A, flavokawain B, and flavokawain C. The ginger CRM contained 6-gingerol, 8-gingerol, 10-gingerol, 6-shogaol, 8-shogaol, and 10-shogaol.
Each phytochemical was sourced as an isolated compound and assigned a purity factor by a mass balance approach accounting for residual impurities. The solution standard mixes were formulated by gravimetric addition of each phytochemical incorporating the purity factor and diluting with acetonitrile to the target concentrations of 500 µg/mL for the gingerols and shogaols, 250 µg/mL for the kavalactones, and 25 µg/mL for the flavokawains.
The concentration accuracy of each component in the solution mixes was analytically verified by ultra high performance liquid chromatography with ultraviolet detection (UHPLC-UV) assay comparison to an independently prepared calibration solution. Each component in the ginger and kava CRMs were within 5 and 7% of the target concentrations, respectively.
Homogeneous kava and ginger phytochemical solution mixes were produced with accurate constituent concentrations and demonstrated good stability over 2 years. These solution mixes were launched as commercially available CRMs.
These mixes can be used as accurate concentration stock solutions to prepare calibrators and controls for botanical dietary supplement product testing and standardization.
源自植物的膳食补充剂因其潜在的健康益处，在生物医学研究中被广泛使用和研究。为了确保产品制备的一致性和研究结果的可重复性，有必要对植物成分中的关键化学成分进行准确鉴定和定量。制造商需要定量参考物质来验证成分和产品的含量。通过对机制、临床和安全性研究中使用的干预措施进行彻底的特征描述，可以提高生物医学研究的严谨性和可重复性。定量参考物质可实现可靠的产品质量评估和可重复的研究结果。
开发了基于溶液的认证参考物质（CRM）混合物，用作姜和卡瓦中植物化学物质的校准标准。卡瓦 CRM 包含醉椒素、去甲氧基醉椒素、二氢醉椒素、DL-卡瓦因、石菖蒲烯、二氢石菖蒲烯、法沃卡宾 A、法沃卡宾 B 和法沃卡宾 C。姜 CRM 包含 6-姜酚、8-姜酚、10-姜酚、6-姜辣素、8-姜辣素和 10-姜辣素。
每种植物化学物质均作为分离化合物获得，并通过质量平衡方法分配纯度因子，该方法考虑了残留杂质。通过重量法添加每种植物化学物质来配制溶液标准混合物，同时加入纯度因子并稀释至目标浓度：500µg/mL 的姜酚和姜辣素、250µg/mL 的卡瓦内酯和 25µg/mL 的法沃卡宾。
通过超高效液相色谱与紫外检测（UHPLC-UV）分析验证了溶液混合物中每个成分的浓度准确性，该分析方法与独立制备的校准溶液进行了比较。姜和卡瓦 CRM 中的每个成分的浓度均在目标浓度的 5%和 7%以内。
制备了均匀的卡瓦和姜植物化学物质溶液混合物，其组成成分浓度准确，且在 2 年内稳定性良好。这些溶液混合物已作为市售 CRM 推出。
这些混合物可用作准确浓度的储备溶液，用于制备植物膳食补充剂产品测试和标准化的校准标准和对照品。
