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Callicarpae Formosanae Folium (CFF), derived from the leaves of Callicarpa formosana Rolfe, is a common Chinese medicinal herb used for the treatment of hematemesis. Phytochemical studies found that phenylpropanoids, flavonoids, terpenoids and polysaccharides were the main ingredients of CFF. However, there is limited scientific information concerning holistic quality method and quality consistency evaluation of CFF. In this study, a strategy integrating HPGPC-ELSD, HPLC-PDA, UV–VIS and UPLC-QTOF-MS/MS was firstly developed to simultaneously qualify and quantify polysaccharides, as well as representative small molecules in CFF. HPGPC-ELSD was applied to characterize the molecular weight distribution of polysaccharides, HPLC-PDA was developed to qualitatively and quantitatively determine monosaccharides. UV-VIS was used to determine the total polysaccharides content, and UPLC-QTOF-MS/MS was established to characterize the small molecules. The quality consistency of commercial CFF (CM-CFF) was also evaluated. It was shown that the relative molecular weights, the compositional monosaccharides and small molecules composition in CM-CFF and self-collected CFF (SC-CFF) samples were similar. A total of 32 small molecules including 6 phenylpropanoids, 7 flavonoids and 19 terpenoids were characterized in CFF. However, the variation was observed in the content of polysaccharides, luteolin, ursolic acid, as well as total contents of terponoids in CM-CFF samples, which implied that the holistic quality of CM-CFF was inconsistent. The results suggested that the proposed evaluation strategy could be applied as a potential approach for the quality control of CFF. And the quality of CM-CFF should be improved by Good Agriculture Practice (GAP) base and standard processing method. [Display omitted] • A strategy was firstly developed to analyze polysaccharide and small molecule in CFF. • Quality consistency of commercial CFF samples was evaluated by the strategy. • The holistic quality variation was observed in commercial CFF samples. [ABSTRACT FROM AUTHOR]

Atractylodis Macrocephalae Rhizoma (AMR) is one of commonly used medicinal and edible herbs in China. It is often sulfur-fumigated during post-harvest processing. Carbohydrates are important active components of AMR. However, it is unknown whether sulfur-fumigation would induce changes on carbohydrates. Here, carbohydrates including polysaccharides, oligosaccharides and free monosaccharides were comprehensively analyzed to characterize the quality changes of sulfur-fumigated AMR. Determination of both homemade sulfur-fumigated AMR samples and commercial samples from market revealed that sulfur-fumigation did not affect molecular weight distribution of polysaccharides, but altered polysaccharides content and its ratios of constituent monosaccharides, especially glucose (Glc) and fructose (Fru), as well as the contents of oligosaccharides DP2–10 and free monosaccharide Fru. Moreover, the variations enhanced with the increasing of residual SO 2 content. The potential transformation mechanisms could be due to the hydrolysis of polysaccharides. The research outcomes could provide a chemical basis for the safety and efficacy evaluations of sulfur-fumigated AMR. [Display omitted] • Multi-chromatographic technology methods were integrated to characterize carbohydrates components of AMR. • Impact of sulfur-fumigation on carbohydrates of AMR was evaluated. • Sulfur-fumigation decreased the content of polysaccharides, whereas increased that of oligosaccharides and free fructose. • The variations of carbohydrates enhanced with the increase of SO 2 residual amounts. • The potential transformation mechanisms might be the hydrolysis of polysaccharides into oligosaccharides and monosaccharides. [ABSTRACT FROM AUTHOR]

Si-Jun-Zi decoction (SJZD) with ginseng as the principal medicinal herb is a traditional Chinese Medicine multi-herb prescription that commonly employed to treat colorectal cancer etc. Previous studies showed that nearly half of the commercial ginseng was sulfur-fumigated, one of the postharvest processing methods that commonly causes sulfur-dioxide (SO 2) residue and chemical composition transformation in medical herbs. In this study, the effect of sulfur-fumigated ginseng on global quality of SJZD was evaluated by UPLC-QTOF-MS/MS based metabolomics and multiple chromatographic techniques based glycomics strategies. For non-saccharides components, sulfur-fumigated ginseng led to the emergence of sulfur-containing derivatives and alteration of saponins and flavonoids in SJZD. For saccharide components, sulfur-fumigated ginseng decreased the total contents and molecular weights of polysaccharides, changed the monosaccharide composition of polysaccharides, and increased the contents of oligosaccharides and free monosaccharides of SJZD. The alterations of SJZD were aggravated with the sulfur-fumigated content of ginseng. Those phenomena might be attributed to 1) sulfur-fumigation caused the generation of sulfur-containing derivatives in ginseng, which further transferred to SJZD, and 2) sulfur-fumigation caused the residue of SO 2 in ginseng, which reduced the pH value and further changed the dissolution of saponins and flavonoids and accelerated the degradation of the polysaccharides to oligosaccharides and/or monosaccharides in SJZD. Furthermore, although storage reduced the SO 2 residue in sulfur-fumigated ginseng, it couldn't recover the alterations of chemical profiles in SJZD. In conclusion, sulfur-fumigated ginseng altered the global quality of SJZD, which promoted that extra attention must be paid during the application of herbal formulas that containing sulfur-fumigated herbs. • Sulfur-fumigated ginseng affected the chemical profiles of Sijunzi decoction (SJZD). • The evaluations were assessed by metabolomics and glycomics strategies. • Non-saccharide and saccharide components in SJZD were altered by fumigated ginseng. • Ginseng in high-extent fumigation showed more serious effect on SJZD. • Storage reduced SO 2 residue but not recovered changes of fumigated ginseng on SJZD. [ABSTRACT FROM AUTHOR]

• UPLC-QTOF-MS/MS based chemical profiling was firstly developed for qualitatively characterizing the Impatiens Caulis sample. • A sensitive UPLC-DAD method was firstly developed to quantify eleven compounds in the Impatiens Caulis sample. • The developed method was integrated to compare the quality consistency of commercial Impatiens Caulis samples. In this study, ultra-high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS/MS) and ultra-high performance liquid chromatography coupled with photo-diode array spectrometry (UPLC-DAD) were firstly integrated to qualitatively characterize the chemical profiles and quantitatively determine the major components in Impatiens Caulis (IC), a Chinese medicinal herb derived from the dried stem of Impatiens balsamina. The qualitative analysis revealed that there was no difference in chemical profiles of twenty commercial IC samples. A total of 45 components were characterized, there in 5 naphthoquinones, 3 coumarins, 5 phenolic acids, 12 flavonoids and 3 other compounds were identified definitely. However, the quantitative results showed a significant difference in these IC samples. In particular, the highest content of total quantified compounds was even 9.49 times of the lowest one. Furthermore, the average contents of these quantified compounds in twenty commercial IC samples had high values of relative standard deviation (RSD) ranged from 15.64% to 98.76%, suggesting a poor quality consistency in these commercial IC samples. Therefore, efficacy related chemical markers as well as the cultivation region, harvest time and/or post-harvest handling of IC should be further investigated for ensuring its quality and efficacy consistency. [ABSTRACT FROM AUTHOR]

[Display omitted] • Multi-chromatographic approaches were integrated to compare chemical profiles between MHD and cSHD. • Polysaccharides and small molecules were qualitatively identical between MHD and cSHD. • The contents of albiflorin, paeoniflorin and alkaloids in MHD were lower than those in cSHD. • The content of polysaccharides in MHD was higher than that in cSHD. Chang-Kang-Fang formula (CKF), a multi-herbs traditional Chinese medicine (TCM) prescription for treating irritable bowel syndrome (IBS), has been clinically applied in the traditional form of mixed-herb decoction (MHD), or in the modern form of combined single-herb decoction (cSHD, so called dispensing granule decoction) in the near decades, but the chemical consistency between the MHD and cSHD is still unknown. Herein, a new strategy by integrating multiple-chromatographic approaches to characterize both polysaccharides and small molecules was developed to compare the chemical consistency between MHD and cSHD. Sixteen small molecules were simultaneously qualified and quantified by UPLC-QTOF-MS/MS, the molecular weight distribution of polysaccharides was characterized by HPGPC-ELSD, while the monosaccharide composition and total saccharides content were determined by HPLC-PDA and UV-VIS, respectively. It was found that the molecular weight range and monosaccharide composition of polysaccharides, as well as the composition of small molecules, were identical between MHD and cSHD. However, the contents of berberine, epiberberine, coptisine, palmatine, albiflorin and paeoniflorin in MHD were significantly lower than those in cSHD, whereas the content of polysaccharides in MHD was higher than that in cSHD, indicating that there is a significant difference in the quality between MHD and cSHD, in particular for the relative contents of major small molecules and polysaccharides. Whether or not these quality variations affect the efficacy and safety of CKF deserves further investigation. [ABSTRACT FROM AUTHOR]