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This study aimed to identify and quantify the primary components in lotus leaf and to explore the hypolipidemic components through spectral-effect relationships and chemometric methods. Utilizing a data-dependent acquisition-diagnostic fragment ion/characteristic neutral loss screening strategy (DFI-NLS), a reliable HPLC-Q-TOF-MS analysis was conducted, identifying 77 compounds, including 36 flavonoids, 21 alkaloids, 3 terpenoids, 11 organic acids, 4 phenols, 1 lignin and 1 unsaturated hydrocarbon. A straightforward HPLC-DAD method was developed for the simultaneous determination of seven major components in lotus leaf, and quercetin-3-O-glucuronide (Q3GA) was identified as the most abundant component. The HPLC fingerprints of 36 lotus leaf sample batches were assessed using chemometric approaches such as principal component analysis and hierarchical cluster analysis. The hypolipidemic effect of these samples was analyzed by measuring total cholesterol (TC) and total triglycerides (TG) levels in palmitic acid (PA) and oleic acid (OA)-induced lipid modeling in HepG-2 cells, employing partial least squares regression and grey relation analysis to investigate the spectral-effect relationship of the lotus leaf. The in vivo hypolipidemic effect of these compounds was assessed using an egg yolk powder-induced high-fat zebrafish model. The findings indicated that peak No.11 (Q3GA) in the chemical fingerprint was significantly associated with hypolipidemic activity, suggesting it as a potential hypolipidemic compound in lotus leaf. In summary, this study facilitates the exploration of the phytochemical compounds and their bioactive properties in the lotus leaf. [Display omitted] • Seventy-seven compounds were comprehensively identified in lotus leaf. • Flavonoids in lotus leaf exhibit significant hypolipidemic activity. • Quercituron is a compound with potent hypolipidemic activity in lotus leaf. [ABSTRACT FROM AUTHOR]

The fruits of Siraitia grosvenorii are considered to be health-promoting because of the diversity of their bioactive ingredients. In the present study, a screening method, using high-performance liquid chromatography/quadrupole-time-of-flight mass spectrometry (HPLC-Q-TOF-MS) combined with a screening strategy, has been established. The technology was used to systematically screening the targeted metabolites, primarily from the complex matrix of S. grosvenorii . The compounds were then identified by their exact masses and characteristic fragment ions, in comparison with the fragmentation behaviors of 19 references. Finally, 122 compounds, including 53 flavonols and flavonol glycosides, 59 triterpene glycosides and 10 siraitic acid glycosides, were screened and identified in 10-, 50- and 80-day fruits, roots, stems and leaves of S. grosvenorii . 98 of them were reported for the first time. Additionally, the distribution of all identified components in different parts of the plant was determined and metabolic networks for flavonol and triterpene glycosides were proposed. [ABSTRACT FROM AUTHOR]

Ursodeoxycholic acid has gained increasing attention due to its recent discovery of the preventive effect on SARS-CoV-2 infection. Ursodeoxycholic acid has been included in various pharmacopoeias as an old drug, and the latest European Pharmacopoeia lists nine potential related substances (impurities A∼I). However, existing methods in pharmacopoeias and literature can only quantify up to five of these impurities simultaneously, and the sensitivity is inadequate, as the impurities are isomers or cholic acid analogues lacking chromophores. Herein, a novel gradient RP-HPLC method coupled to charged aerosol detection (CAD) was developed and validated for the simultaneous separation and quantification of the nine impurities in ursodeoxycholic acid. The method proved sensitive and allowed the quantification of the impurities as low as 0.02 %. Relative correction factors of the nine impurities were all within the range of 0.8–1.2 in the gradient mode by optimizing chromatographic conditions and CAD parameters. In addition, this RP-HPLC method is fully compatible with LC-MS due to the volatile additives and high percentage of the organic phase, which can be directly used for the identification of impurities. The newly developed HPLC-CAD method was successfully applied to commercial bulk drug samples, and two unknown impurities were identified by HPLC-Q-TOF-MS. The effect of CAD parameters on the linearity and correction factors was also discussed in this study. Overall, the established HPLC-CAD method can improve the methods in current pharmacopoeias and literature and contributes to understanding the impurity profile for process improvement. [Display omitted] • Separation of all nine specified impurities of ursodiol by a single method. • HPLC with charged aerosol detector to detect impurities for lack of chromophores. • Method proved sensitive and correction factors of nine impurities were all 0.8–1.2. • Method is compatible with LC-MS and two unknown impurities were identified. • Overcoming the deficiency of existing methods in pharmacopoeias and literature. [ABSTRACT FROM AUTHOR]

Yihuang decoction (YHD) is one of the most famous formulas in tradition Chinese medicine (TCM) and has been clinically used for treatment of vaginitis, pelvic inflammation and other gynecological diseases for hundreds of years. However, its chemical composition remains unclear. In this study, high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MS) was employed for its chemical profiling investigation. As a result, 90 components were chemically defined, including 23 alkaloids, 14 organic acids, 3 phenylethanoid glycosides, 4 iridoid glycosides, 5 terpenoid lactones, 10 flavonoids, 8 nucleobases and nucleosides, 12 amino acids, and 11 other compounds. In addition, 8 representative compounds (acteoside, allantoin, berberine, 4- O -feruloylquinic acid, 5- O -feruloylquinic acid, gallic acid, geniposidic acid, and phellodendrine) were simultaneously determined in 10 batches of YHD samples by HPLC with a diode array detector (HPLC-DAD). For all the analytes, their calibration curves showed good linearity (R2 >0.9990) within the test ranges. RSDs of precision, repeatability and stability test were all below 3.50%. The overall recoveries ranged from 93.63% to 105.02%, with RSDs less than 3.50%. This study is supposed to exhibit a comprehensive chemical profiling of YHD and to provide some strong basis for quality control and even for action mechanism of this ancient classical prescription. [Display omitted] • The chemical profiling of YHD was elucidated by HPLC-Q-TOF-MS. • Totally 90 compounds have been identified in YHD. • 8 representative compounds in 10 batches of YHD were simultaneously quantified by HPLC-DAD. [ABSTRACT FROM AUTHOR]

A high-performance liquid chromatography (HPLC) method has been developed for the determination of related substances in egg yolk lecithin. Chromatographic separation was achieved using a gradient elution on a Waters Xbridge HILIC column maintained at 35 ℃. Mobile phase A was composed of water-acetonitrile (80:20, v/v, containing 5 mM ammonium acetate), and mobile phase B was composed of acetonitrile. Analytes were monitored by a charged aerosol detector (CAD) at 50 ℃. The novel HPLC-CAD method was selective and sensitive for the determination of related substances in egg yolk lecithin in its commercial bulk batches. It was also successfully validated by the International Council for Harmonisation (ICH) guidelines. The method will be a renewal of an old Chinese Pharmacopoeia method (2020 edition). Moreover, quadrupole time-of-flight mass spectrometry (Q-TOF-MS) was integrated with HPLC to investigate phospholipid species in egg yolk lecithin. This work provides comprehensive composition profiles of egg yolk lecithin, thereby accelerating the quality control, development, and application of egg yolk lecithin. [Display omitted] • Determination of related substances in egg yolk lecithin was developed and validated with HPLC-CAD. • In the profile of egg yolk lecithin, 121 phospholipid molecules were identified using HPLC-Q-TOF-MS. • This proposed method is selective, efficient, sensitive, and QC-friendly for routine analysis of related substances in egg yolk lecithin. [ABSTRACT FROM AUTHOR]