College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
J Pharm Biomed Anal. 2022 Sep 5;218:114842. doi: 10.1016/j.jpba.2022.114842. Epub 2022 May 20.
Corni Fructus (CF), used for thousands of years in Asia as food and medicine, has different therapeutic effects before and after processing. In the past work, the quality assessment of Corni Fructus focused on the limited chemical compounds and rarely correlated external properties, such as color. The traditional sensory assessment relies partly on human eyes, which is quick but lacks objectivity. On a Shimadzu LC-20AD liquid chromatograph system equipped with a diode-array detector (DAD), we determined six major compounds (gallic acid, 5-hydroxymethyl-2-furaldehyde, morroniside, loganin, sweroside, and cornuside I). The extract was analyzed using ultra-high-performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry (UHPLC-QTOF-MS) after the solid-phase extraction (SPE) step. Totally 58 compounds in raw and processed Corni Fructus were identified in negative and positive ion modes according to tandem mass spectrometry (MS/MS) fragments. Iridoids, carboxylic acids, tannins, flavonoids, triterpenes, fatty acids, saccharides, phospholipids, polysaccharide, amino acid, amide, furan, catechol, aldehyde, fatty alcohol and vitamin were included. A multivariate statistical analysis based on UHPLC-QTOF-MS filtered 17 differential compounds between raw and processed products. The CM-5 colorimeter was applied for digitizing surface and powder color. The contents of gallic acid, morroniside, loganin, cornuside I, and sweroside significantly correlated with color parameters in raw Corni Fructus, particularly a* and b* , but not in processed products, according to Spearman correlation analysis. MS peak area of four compounds in raw products correlated significantly with color parameters L* , a* , b* , L* , a* , b* , respectively, while three compounds in processed products with L* , a* , b* . It revealed the relationship between compounds and color of Corni Fructus and the crucial compounds to color. In this study, we successfully developed a method for comprehensive quality evaluation of Corni Fructus that combines HPLC, UHPLC-QTOF-MS, and color determination.
山茱萸(CF)在亚洲被用作食物和药物已有数千年的历史,其炮制前后具有不同的治疗效果。在过去的工作中,山茱萸的质量评估主要集中在有限的化学化合物上,很少与外部性质相关联,例如颜色。传统的感官评估部分依赖于人的眼睛,虽然快速但缺乏客观性。在配备二极管阵列检测器(DAD)的岛津 LC-20AD 液相色谱系统上,我们测定了六种主要化合物(没食子酸、5-羟甲基-2-糠醛、莫诺苷、马钱苷、獐牙菜苷和山茱萸苷 I)。提取物在固相萃取(SPE)步骤后,使用超高效液相色谱-四极杆飞行时间串联质谱(UHPLC-QTOF-MS)进行分析。根据串联质谱(MS/MS)片段,在生品和炮制品中总共鉴定出 58 种化合物。包括环烯醚萜类、羧酸类、鞣质类、黄酮类、三萜类、脂肪酸类、糖类、磷脂类、多糖类、氨基酸类、酰胺类、呋喃类、儿茶酚类、醛类、脂肪醇类和维生素类。基于 UHPLC-QTOF-MS 的多变量统计分析筛选出生品和炮制品之间的 17 种差异化合物。采用 CM-5 测色仪对表面和粉末颜色进行数字化。生山茱萸中,没食子酸、莫诺苷、马钱苷、山茱萸苷 I 和獐牙菜苷的含量与颜色参数(尤其是 a* 和 b*)显著相关,但炮制品中不相关,根据 Spearman 相关分析。生品中四种化合物的 MS 峰面积与颜色参数 L*、a*、b*、L*、a*、b分别显著相关,而三种化合物与 L、a*、b*相关。这揭示了山茱萸中化合物与颜色的关系以及对颜色有重要影响的关键化合物。在这项研究中,我们成功地建立了一种结合 HPLC、UHPLC-QTOF-MS 和颜色测定的山茱萸综合质量评价方法。