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더덕(Codonopsis lanceolata)은 주로 한국, 중국 등 동아시아 지역에 재배되고 있으며, 더덕의 뿌리는 기침, 기관지염, 천식, 결핵, 소화 불량의 증상을 치료하기 위한 기능성 식품 및 전통 의학으로 사용되어져 왔다. 보고된 바에 의하면 phenylpropanoids, polyacetylenes, saponins, flavonoids와 같은 다양한 식물 천연물 성분들이 항비만, 항염, 항암, 항산화, 항미생물 활성과 같은 약리학적 작용에 관여한다고 보고되어 있다. MS기반 대사체학 분석을 이용한 주산지의 마커 성분을 선정하는 것은 다른 지역에서 재배된 약용 식물의 안전성뿐만 아니라 화학적 조성과 생물학적 효능의 변화와도 관련이 있기 때문에 부작용 없이 더덕의 유익한 효과만을 보장하는데 중요하다. 본 연구에서는 국내산 더덕의 주산지 특성을 구별하기 위해 UPLC-QTOF-MS를 기반으로 하는 대사체 프로파일링과 다변량 통계분석 기법인 PCA 분석을 수행하여 판별모델을 확립하였다. 그 결과 인제(강원도), 횡성(강원도), 무주(전라북도)의 3개 그룹이 PCA와 loading plot 분석결과 tangshenoside I, lancemaside A, lancemaside G는 더덕 주산지를 구별하기 위한 잠재적 대사체 마커들로 제안하였다.

Macamides are characteristically found in maca (Lepidium meyenii Walper). Fatty acid derivatives are also an important type of constituent in maca, since they not only relate to the biosynthesis of macamides in the postharvest process but also possess some bioactivities. To study their comprehensive profiles in maca tubers processed via the air-drying method, ultraperformance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) analyses were performed to identify macamide and fatty acid molecules. Their contents in maca tubers that were processed via air drying and freeze drying, respectively, were further quantified using high-performance liquid chromatography (HPLC) analyses comparing with eight macamide and three fatty acid reference standards. A total of 19 macamides (including four novel ones) and 16 fatty acid derivatives (two found in maca for the first time) were identified. Quantification analyses results showed the eight macamides with contents ranging from 31.39 to 1163.19 μg/g (on dry tuber), and fatty acids from 18.71 to 181.99 μg/g in the air-dried maca, but there were only three macamides and one fatty acid detected with very low contents (3.97–34.36 μg/g) in the freeze-dried maca. The results demonstrated that the air-drying method can increase the accumulations of macamides and fatty acids in the metabolism of maca in the postharvest process. The biosynthesis of two types of macamides, i.e., N-benzyl-oxo-octadecadienamides and N-benzyl-oxo-octadecatrienamides, was further elucidated in detail. These results provide more valuable insights into the phytochemicals of maca, which is helpful to explain its health benefits.

Background: The activation or overexpression of histone deacetylases (HDACs) are associated with the development of numerous cancers. The importance of HDACs in new anticancer therapeutic strategies has led researchers to develop promising anticancer drugs, design, and synthesis of novel HDACs inhibitors are also in progress. E14 was synthesized and acted as a selective inhibitor of HDACs I. Methods: We develop a sensitive UPLC-QTOF-MS/MS method to discover the new phase Ⅰ and Ⅱ metabolites of E14 from complex biological matrices in plasma, feces and urine of rats. Then a strategy comparing samples after administration with blank samples was applied to distinguish metabolites. The accurate measurements of the product ions obtained by high-resolution mass spectrometry, the structure of the parent drug and its detected metabolites are used to verify its fragmentation pathway and to obtain the proposed structure of the metabolites. Results: Fourteen metabolites were tentatively identified, including twelve metabolites in urine, five in plasma and one metabolite in feces. Hydroxylation, oxidation, methylation, N-demethylation, dehydration, glucuronidation, dehydroxylation and hydrolysis were the main metabolic pathways of E14. Conclusion: E14 is a drug with a variety of metabolites and metabolic pathways. E14 metabolites was excreted most in urine, indicating the main metabolic organ was kidney.

올리브 (Olea europaea L.) 잎은 풍부한 폴리 페놀을 함유하고 있으며, 이는 항산화, 항균, 항 바이러스, 항암 활성을 연관시키고 혈소판 활성화를 억제하는 것으로 보고 되어있다. 올리브 잎은 건강기능성식품 및 기능성 화장품의 원료로 상업적으로 사용되고 있으며, 이러한 건강상의 이점은 올리브 잎의 주요 생리활성 물질인 oleuropein와 관련이 있다. Oleuropein은 항산화, 항노화, 항염증, 항암, 항미생물, 항바이러스, 항죽상동맥혈증, 지질 저하 효과, 혈당 저하 효과, 피부 보호 효과가 보고되어 있다. oleuropein이 올리브 잎의 중요한 화합물 임에도 불구하고 상업용 제품에서 oleuropein 함량을 밝히는 정량적 접근 방법은 아직 없다. 본 연구에서는 UPLC-QTof/MS, PDA, CAD로 개발된 방법을 이용하여 10개의 상업용 올리브 잎 추출물의 성분 및 oleuropein 함량을 분석 하였다. Iridoids (1, 3, 4, 14, and 16-18), coumarin (2), phenylethanoids (5, 9, and 11), flavonoids (6-8, 10, 12, and 13), lignan (15)을 포함한 총 18종의 화합물이 올리브 잎에서 예상되었다. 총 10종의 올리브 잎 추출물 분석은 3종의 제품(A, G, H)에서 제품에서 제시한 oleuropein 함량보다 높게, 5종의 제품(B, E, H, I, J)에서 5-10%의 오차범위로 나타났고 C, D에서 함량 미달로 검출되었다. 본 연구에서 oleuropein의 함량분석이 올리브 잎의 품질 관리에 도움이 될 수 있음을 판단하였다.

Honey maturity is an important factor in evaluating the quality of honey; however, there are few studies on the molecular mechanism of the formation of mature honey (MH). In this study, the different metabolites of stomach honey (SH), immature honey (IMH), and MH samples during the same rapeseed flower season were analyzed by an UPLC-QTOF-MS-based metabolomics approach. MH was found to have a distinct metabolic profile to IMH, and a total of 9 different metabolites were obtained, 3 of which, including decenedioic acid, were accumulated in MH. Decenedioic acid as a bee-originated fatty acid (FA) was further verified in rape, acacia, and jujube honey by GC-MS, making it a potential marker to discriminate IMH and MH (P < 0.01). Besides, MH showed higher FAs concentrations; in particular, 3 FAs were significantly richer in MH than IMH (P < 0.05). This study reveals the molecular mechanism from IMH to MH from a FA perspective.

Background End-stage renal disease (ESRD) is the final stage during the development of renal failure. Depression is the most common psychiatric disorder in patients with ESRD, which in turn aggravates the progression of renal failure, however, its underlying mechanism remains unclear. This study aimed to reveal the pathogenesis and to discover novel peripheral biomarkers for ESRD patients with depression through metabolomic analysis. Methods Ultra-high-performance liquid chromatography coupled with mass spectrometry (UPLC-MS) was used to explore changes of serum metabolites among healthy controls, ESRD patients with or without depression. The differential metabolites between groups were subjected to clustering analysis, pathway analysis, receiver operating characteristic (ROC) curve analysis. Results A total of 57 significant serum differential metabolites were identified between ESRD patients with or without depression, which were involved in 19 metabolic pathways, such as energy metabolism, glycerolipid metabolism, and glutamate-centered metabolism. Moreover, the area under the ROC curve of gentisic acid, uric acid, 5-hydroxytryptamine, 2-phosphoglyceric acid, leucyl-phenylalanine, propenyl carnitine, naloxone, pregnenolone, 6-thioxanthene 5'-monophosphate, hydroxyl ansoprazole, zileuton O-glucuronide, cabergoline, PA(34:2), PG(36:1), probucol and their combination was greater than 0.90. Conclusions Inflammation, oxidative stress and energy metabolism abnormalities, glycerolipid metabolism, and glutamate-centered metabolism are associated with the pathogenesis of ESRD with depression, which may be promising targets for therapy. Furthermore, the identified differential metabolites may serve as biomarkers for the diagnosis of ESRD patients with depression.

The wild plant Campanumoea lancifolia (Roxb.) Merr (also called Hong Guo ginseng, HGG), is naturally distributed in a Hmong minority area in western Hunan Province, China. The objective of this study was to identify, quantify, and elucidate the polyphenols and anthocyanins, and their antioxidant activities (via 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical and 2,2��-azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radical cation scavenging abilities) tested in vitro in the whole fruit, fruit skin, fruit pulp, and leaves of the plant. Results showed that Total polyphenol content (TPC) was highest in leaves (97.76 mg/g), followed by whole fruit (18.18 mg/g), fruit skin (26.16 mg/g), and fruit pulp (8.99 mg/g). Total anthocyanin content (TAC) in fruit skin was the highest at 27.44 mg/g, compared with leaves (20.18 mg/g), whole fruit (12.94 mg/g), and fruit pulp (4.36 mg/g). DPPH scavenging ability and ABTS scavenging ability test followed a decreasing order with the highest ability in leaves, fruit skin, whole fruit, and fruit pulp. Main phenolic compounds (chlorogenic acid, rutin, luteolin-7-O-glucoside, and apigenin) were also highest in leaves. Phenolic compounds and anthocyanins in whole fruit and leaves were further identified using UPLC-QTOF-MS, resulting in the identification of six phenolic acids and their derivatives, seventeen flavonoids and their derivatives, and two anthocyanins observed. These results thus provide the phytochemical evidence to explain and understand the medical and health benefits of HGG.

Tibetan hulless barley (“qingke” in Chinese) is a valuable food in Tibet. Purple qingke (PQK) and black qingke (BQK), two special pigmented types of hulless barley, have traditionally been widely cultivated and consumed in Tibet for thousands of years. The composition and contents of anthocyanins of two cultivars are unknown. This study aimed to explore the composition and contents of anthocyanins of two cultivars and their antioxidant capacities. Six anthocyanins were identified by ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry from barley, most of the anthocyanins were acylated by malonyl group. The total anthocyanin contents ranged from 141 to 2,304 μg/g in PQK and from 248.7 to 2902.9 μg/g in BQK. Furthermore, qingke has strong antioxidant activity against DPPH, ABTS˙+, and FRAP. Qingke may be useful for treating or preventing diseases caused by the overproduction of radicals.

Phyllostachys edulis (PES), the most important bamboo species in China, is widely distributed in East Asia. Flavonoids, which are important bioactive natural compounds, often have similar structures, making their structural elucidation difficult. The aim of this study was to represent valuable, reliable mass spectral data for the identification of flavonoids in plant leaves. Ultra-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (UPLC–Q-TOF-MS/MS) method was established for characterization and identification of the major flavonoids in PES leaf extract. A total of 13 flavonoids were simultaneously characterized, and their proposed characteristic product ions and fragmentation pathways were investigated. Thirteen compounds were separated on an Agilent Zorbax RRHD SB-C18 column (150 mm × 2.1 mm, 1.8 μm). On the basis of comparing with the 4 reference standards and the literature data, the other 9 flavonoids were identified by tandem mass spectrometry (MS/MS). Eight compounds (compounds 1, 4, 5, 8, 9, 10, 11, and 12) were found in PES leaves for the first time. An efficient UPLC–QTOF-MS/MS method was successfully applied for the structural identification of flavonoids in PES leaves. These results have practical applications for the rapid identification and structural characterization of these compounds in crude bioactive extracts or mixtures.

Blackberry fruit (Rubus spp. L., Rosaceae) is a source of natural antioxidants for cosmetic products due to its abundance of phenolic compounds. The aim of the present study was to characterize blackberry extracts of the cultivars ‘Tupy’, ‘Guarani’, and ‘Xavante’ and to develop niosomes loaded with blackberry extracts for future applications in cosmetic formulations. After fruit collection at the Experimental Central Stations of the Federal University of Parana, Quatro Barras, Brazil, the extracts were solubilized in different solvents. The choice of extraction solvent and blackberry cultivar was established by analysis to evaluate the total phenolic content, radical scavenging capacity, and chemical characterization by ultra-performance liquid chromatography couple to quadrupole time-of-flight-mass spectrometry. These tests revealed that fruits of Rubus ‘Xavante’ had the highest potential to be used as an active cosmetic ingredient. Niosomes formulated with the acetone/water extract obtained from the fruit of this cultivar showed both good performance and encapsulation efficiency. The results indicate that this type of niosome can be considered a promising delivery system with the potential to improve skin absorption, in addition to the antioxidant, anti-aging, and UV protective activities of the polyphenol-rich blackberry extracts.

Yinqiaosan is a classic Chinese herbal medicine formula that has been used to treat various bacterial and viral infections by Chinese medicine doctors for over two centuries. In this work, we developed a comprehensive qualitative and quantitative method for identification, quantitation, and quality assessment of chemical constituents of Yinqiaosan formula in four different preparation forms (i.e., decoction, granule, pill, and tablet), which employed ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry with a single exogenous reference internal standard for untargeted metabolomics profiling and global semiquantitative analysis. The use of a single exogenous reference internal standard permitted not only qualitative and quantitative analyses of multiple herbal components in a single instrument run, but also cross-comparison of chemical contents in between all four Yinqiaosan preparation forms. The acquired mass chromatograms were analyzed, quantitated, and compared using multivariate data analysis for similarities and differences of chemical constituents in four Yinqiaosan preparation forms. For the first time, we were able to identify over 100 chemical constituents from each preparation form using the available database. Among the 49 commonly identified compounds in the 4 Yinqiaosan preparation forms, 16 have been reported to have pharmacological activities, which may be used in a network pharmacology study of Yinqiaosan for exploring the underlying mechanism of the herbal formula.

Background Neonatal acne occurs in the first few weeks after birth. Some lesions are more serious and leave scars. Maternal surface skin lipids (SSL) have a strong correlation with SSL of infants. The establishment of prediction rank model based on maternal SSL is essential to the prevention and treatment of neonatal acne. Method Surface skin lipids samples were collected from the mothers (M) of 56 neonatal acne patients and the mothers (HM) of 19 healthy infants. Surface skin lipids from the right forehead were collected using a noninvasive method. UPLC-QTOF-MS was applied to detect SSL. Partial least squares discriminant analysis and receiver operating characteristic (ROC) analysis were performed to screen and validate potential lipids. Random forest (RF) and ROC analysis were used to establish a prediction model and evaluate its accuracy. Results Sixteen altered potential lipids belonging to fatty acids, sphingomyelins, and glycerides were associated with M. M had less lipids than HM. Spearman's correlation of 16 lipids revealed 9 with high correlation. They were chosen as characteristic values of the RF prediction model. And the model showed an average accuracy of 98% in the validation set. Conclusion We have established an RF model for predicting neonatal acne and have shown that high skin barrier-related lipids were markers for predicting neonatal acne.

Jilin Province and Shandong Province are two main American ginseng (AG) producing areas in China. The geographical difference existed in these two provinces. Aiming at evaluating the similarities and differences of the secondary metabolites, the comprehensive metabolite profiling of AG from Jilin Province (AG

The stem rot disease has emerged globally as a major disease threat to the productivity and seed quality of oilseed Brassica. The generalist causal pathogen Sclerotinia sclerotiorum (Lib.) de Bary shows large variability in their aggressiveness and pathogenicity. Revealing the metabolic profile and signaling components of the pathogen in host-pathogen interaction are fundamental in understanding host resistance to the disease. In this study, the metabolites released by the pathogenic strains of S. sclerotiorum under the axenic culture have been identified using the untargeted high-resolution UPLC-QTOF-ESI-MS/MS. The analysis of the ethyl acetate extracts of the S. sclerotiorum culture revealed ten major secondary metabolites namely, sclerin, sclerotinin-B, sclerone, melanin, bostrycoidin, botcinin-D, botcinin-A, gliovirin, scleramide, and botcinic acid. The later six metabolites are being reported for the first time in the culture extract of the S. sclerotiorum pathogen. The phylogenetic analysis based on the overlapping and unique informative peaks in the chromatograms, the six S. sclerotiorum strains were grouped into three major clads. The clustering based on metabolic profiles does not substantiate the diversity based on morphology or virulence differences on the host. The findings of the study signified the metabolites secreted under the axenic conditions are varies based on their growth and developmental stages and may not necessarily be the determining factors for their differential aggressiveness and virulence over the host.

Many species from the genus Citrus are used in traditional medicine and contain polymethoxylated flavonoids. These compounds show anti-inflammatory and chemopreventive activities, among others, and therefore have a big potential to be developed as therapeutic agents or dietary supplements. Citrus species are different in their profile and yield of polymethoxylated flavonoids. Therefore, polymethoxylated flavonoids were identified and quantified in seven different Citrus species, including wild-type and commercially available species. All species were profiled using UPLC-QTOF-MS/MS analysis combined with mass spectral molecular networking. A total of 38 polymethoxylated flavonoids were detected and 8 of them were present in every species. As the yield of polymethoxylated flavonoids was different for each species, a generally applicable HPLC-diode array detection method was developed and validated according to the ICH guidelines to quantify the amount of nobiletin and the total amount of polymethoxylated flavonoids expressed as nobiletin. Analysis of the seven samples showed evidence that wild-type Citrus species (e.g., Citrus depressa) contain higher yields of polymethoxylated flavonoids compared to commercially available species (e.g., Citrus limon). Qualitative analysis revealed the broadest variety of different PMFs in C. depressa, Citrus reticulata, and Citrus reticulata × Citrus sinensis, which makes them interesting sources of polymethoxylated flavonoids for future development as therapeutic agents or dietary supplements.

The preventive and therapeutic effects of dark tea fermented by Eurotium cristatum (DTE) in glucose metabolism have been demonstrated. However, few studies have investigated comprehensive changes in the chemical composition and activity in DTE before and after fermentation. In this study, the metabolic profiling of raw samples and fermented samples was determined by ultra-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS/MS). Furthermore, a systematic analytical strategy combining global metabolomics and the spectrum-effect relationship based on α-glucosidase inhibition was employed for screening discriminant metabolites. As a result, 15 discriminant metabolites were identified in DTE samples. Among them, 10 metabolites (4 fatty acids, 1 dyphylline derivative, 3 lysophosphatidylcholines, and 2 triterpenes) increased in relative contents and the contents of the other 5 polyphenol metabolites decreased after fermentation. These metabolites were critical constituents possibly associated with DTE's hypoglycemic activity, which also might be suitable as quality evaluation indicators. This study provided a worthy insight into the exploration of representative active constituents or quality indicators of DTE.

In this study, based on depolymerization solution of commercially available sodium lignosulfonate under mild conditions, an efficient method for the chromatographic separation of lignosulfonate depolymerization products was firstly established. The self-built database contains 18 lignin-based standards and the information on their names, formulas, structures, retention times, fragments, and corresponding MSE data was developed. By searching the online spectral data in a novel informatics database, a total of nine aromatic lignin depolymerization products were identified automatically. Thus, a fast standard protocol for detection and identification of real lignin degradation products was preliminary built.

The residue of antibiotics in meat and meat products is one of the social problems for its effects and risks to human health, especially in the antibiotic resistance crisis. Nowadays, there are hundreds of drugs commercially available, with difference biochemical characteristics. Therefore, it is necessary to determine and monitor these residues in meat and meat products. The methods using liquid chromatography (LC) and ELISA are widely applied in numbers of laboratories to determine specified substances. In several laboratories, the state-of-the-art highresolution analytical technique, using Ultra Performance Liquid chromatography-triple quadrupole Time-of-flight mass spectrometry (UPLC-QTOF-MS), is applied to analyse the knowns and unknowns residues in food. In this study, we used this technique for screening the residue of antibiotics, banned substances (Sulfonamids, Quinolones, Tetracyclines, β-Agonists…) and other toxins in pork, chicken, beef and fish samples. Ninety-three randomly collected samples have been screened and residues of Amoxicillin, Cefalexin and Ampicillin have been detected in three of them.

Schizonepetae Spica (SS), a well-known traditional Chinese medicine has been widely used over thousands of years. In modern medicine, it has been adopted in the traditional prescription for cancer ...

A-type epigallocatechin-3-gallate (EGCG) and epicatechin-3-O-gallate (ECG) dimers have multiply biological activities. In this study, the pharmacokinetics of them were investigated in mice after a single dose intravenous administration, and the metabolites in mice plasma and urine were investigated by ultra-performance liquid chromatography-Quadrupole-time of flight mass spectrometer (UPLC-QTOF-MS). Our results showed that the half-life (

The valorization of residual forest biomass from sawmills is an economic and ecological opportunity in Quebec. With specialized metabolites and biological activities, several residues from...

Objective: This study was conducted to develop an method for identification of Trachemys scripta elegans (Ba Xi Gui, 巴西龟) shell glue from Chinemys reevesii (Zhong Hua Cao Gui, 中华草龟) shell glue. Methods: In this research, an ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-QTOF/MS) method coupled with Binary Compare tool of UNIFI software was validated to differentiate Trachemys scripta elegans (Ba Xi Gui, 巴西龟) shell glue from Chinemys reevesii (Zhong Hua Cao Gui, 中华草龟) shell glue. The gelatins were digested enzymatically into peptides using trypsin.The UPLC-QTOF/MS data of the trypsin digested samples was subjected to Binary Compare of UNIFI software in order to screen out the unique peptides. PEAKS® Studio software was utilized to identify the sequence of the marker peptides. Results: It was found that m/z 641.3 was the marker peptide in samples of Trachemys scripta elegans (Ba Xi Gui, 巴西龟) shell glue, and m/z 649.3 was the marker peptide in samples of Chinemys reevesii (Zhong Hua Cao Gui, 中华草龟) shell glue, with possible amino acid sequence of GEAGPSGPAGPTGAR and GESGPSGPAGPTGAR respectively. Conclusions: The results will be helpful for the differentiating between these 2 gelatins, and it can be also used for quality control of Tortoise shell glue (Gui Jia Jiao, 龟甲胶). Keywords: UPLC-QTOF/MS, Tortoise shell glue, Trachemys scripta elegans (Ba Xi Gui, 巴;西;龟), Chinemys reevesii (Zhong Hua Cao Gui, 中;华;草 龟)

Many species of velvet antler have been used as traditional medicine for thousands of years; however, as medicinal materials, velvet antler derived from different animals have different clinical effects. To distinguish the differences and homologies, ultra-performance liquid chromatography-quadruple-time of flight mass spectrometry (UPLC-QTOF-MS) coupled with principal component analysis (PCA) was developed and applied to identify these antler samples derived from Cervus nippon Temminck, Cervus elaphus Linnaeus and Rangifer tarandus Linnaeus, which were first tested and compared at the molecular level of protein. The UPLC-MS data of the trypsin digested samples were subjected to PCA, and the potential markers based on peptide were depicted to illustrate their differences. With the integrated strategy combining UPLC-QTOF-MS with PCA, the results from this study indicated that the proposed methods could be successfully applied to distinguish reindeer antler from sika deer antler and red deer antler, which were prescribed in the Chinese Pharmacopoeia (2015 edition).

Flos Carthami, the dried flower of Carthamus tinctorius L. (Compositae), is among the most popular traditional Chinese medicines due to its diverse biological activities such as anticoagulation, vasodilation, antihypertension, antioxidation, neuroprotection, melanin production inhibition, immunosuppression and antitumor activity. At present, Carthamus tinctorius L. is cultivated in various regions under diverse environmental conditions which has led to quality instability of Flos Carthami in the market and may in turn influence its therapeutic efficacy. So it is necessary to characterize the chemical profiles of different geographical origins of Flos Carthami and find differential metabolites contributing to this difference. In this study, a UPLC-QTOF/MS method was developed to characterize chemical differences of Flos Carthami collected in the Xinjiang Uygur Autonomous Region and Henan, Gansu and Yunnan provinces, China. Principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA) were used to differentiate Flos Carthami samples cultivated in the above-mentioned regions. 32 differential metabolites accountable for such variations were identified through variable importance in the projection (VIP). Grey correlation analysis (GCA) was conducted between 32 differential metabolites and climate factors. Climate factors such as XASD, XRH, XHTJ and XATJ had higher significant correlation with most differential metabolites. Conversely, lower significant correlations were observed between climate factors such as XLTA and XATA and the 32 differential metabolites. So, in order to improve the stability of the chemical quality and guarantee the clinical use of Flos Carthami, its phytogeographical variation cannot be neglected and the differential metabolites could be used to guide the quality control of Flos Carthami.

CRP (Citri Reticulatae Pericarpium), a famous traditional Chinese medicine, has also been extensively used in foods and condiments in dietary practice for centuries. According to the Chinese Pharmacopeia (2015 edition) it contains two subtypes, Guangchenpi (GCP) and Chenpi (CP). GCP exclusively originates from the pericarp of Citrus reticulata ‘Chachi’ cultivar and it's generally believed that GCP has superior qualities compared with the other main cultivars (CP). In the present study, an integrated approach combining LC-QTOF MS-based untargeted metabolomics analysis and DNA barcoding molecular identification was conducted to study the genetic diversity and chemical differences between GCP and CP. A validated UPLC-QTOF MS metabolomics method was established to identify markers by using PCA and OPLS-DA models. 34 identified metabolites could be used as chemical markers to distinguish effectively between the two subtypes. Among them polymethoxyflavones (PMF) such as hexamethoxyflavone (nobiletin and natsudaidain), pentamethoxyflavone (tangeretin and sinensetin), and tetramethoxyflavone are the most influential markers. Support vector machines were employed to classify all the samples and these markers showed good prediction accuracy (100%). The results of DNA barcoding showed that the secondary structure of the ITS2 sequences were significantly different among GCP and other three cultivars. The study indicated the integrated method could be a powerful and reliable analytical tool for differentiating GCP from CP.

Panax ginseng exerts good neuroprotective activity at the cell and animal level, but the specific bioactive compounds and action mechanism are needed to be investigated, verified, and confirmed. In this work, affinity ultrafiltration (AUF), UPLC-QTOF-MS, and molecular docking were integrated into one strategy to screen, identify, and evaluate the bioactive compounds in ginseng at the molecular level. Three biological macromolecules (AChE, MAO-B, and NMDA receptor) were selected as the target protein for AUF-MS screening for the first time, and 16 potential neuroactive compounds were found with suitable binding degree. Then, the bioactivity of ginseng and its components were evaluated by AChE-inhibitory test and DPPH assay, and the data indicate that ginseng extract and the screened compounds have good neuroactivity. The interaction between the three targets and the screened compounds was further analyzed by molecular docking, and the results were consistent with a few discrepancies in comparison with the AUF results. Finally, according to the corresponding relation between component-target-pathway, the action mechanism of ginseng elucidated that ginseng exerts a therapeutic effect on AD through multiple relations of components, targets, and pathways, which is in good accordance with the TCM theory.

Tricin, one of the flavones present in edible Poaceae species, was shown to interfere with intestinal inflammatory-related carcinogenesis and suppress metastasis in colon cancer mice models. Those botanical foods and medicinal herbs which contain high content of tricin may be considered as health supplements for colon health. Hence, the present study aimed to identify and quantify the content of tricin in various medicinal herbs, edible botanicals and some agricultural by-products by LC-MS. A list of “top 10 tricin-rich botanicals/medicinal herbs” was built. From the results, the top three high tricin content botanicals are the dried culms of Triticum aestivum (wheat straw), dried culms of Oryza sativa (rice straw) and mature fruits of Imperata cylindrica. Furthermore, a simple, straightforward isolation method has been developed to isolate tricin from wheat straw which achieved 50% isolation rate (percentage yield of 0.05% w/w) with purity of not less than 98%.

Honey consumption is attributed to potentially advantageous effects on human health due to its antioxidant capacity as well as anti-inflammatory and antimicrobial activity, which are mainly related to phenolic compound content. Phenolic compounds are secondary metabolites of plants, and their content in honey is primarily affected by the botanical and geographical origin. In this study, a high-resolution mass spectrometry (HRMS) method was applied to determine the phenolic profile of various honey matrices and investigate authenticity markers. A fruitful sample set was collected, including honey from 10 different botanical sources (n = 51) originating from Greece and Poland. Generic liquid–liquid extraction using ethyl acetate as the extractant was used to apply targeted and non-targeted workflows simultaneously. The method was fully validated according to the Eurachem guidelines, and it demonstrated high accuracy, precision, and sensitivity resulting in the detection of 11 target analytes in the samples. Suspect screening identified 16 bioactive compounds in at least one sample, with abscisic acid isomers being the most abundant in arbutus honey. Importantly, 10 markers related to honey geographical origin were revealed through non-targeted screening and the application of advanced chemometric tools. In conclusion, authenticity markers and discrimination patterns were emerged using targeted and non-targeted workflows, indicating the impact of this study on food authenticity and metabolomic fields.

The current data report describes the predictive identification of phytochemical constituents in the bioactive extract of Ipomoea mauritiana (IM) whole plant. For several formulations this plant was commonly used as ‘Vidari’ for Ayurvedic medicine. Traditionally, IM tubers are used to alleviate spinal cord pain, improve breast milk, as a tonic, increase sperm count and treating jaundice. The methanol extract can potentially scavenge free radicals and possess antibacterial activity that could be correlated with its chemical composition. So it is crucial to identify the major compounds of IM. An ultra-performance liquid chromatography coupled electrospray ionization quadrupole time-of-flight mass spectrometry (UPLC-ESI-QTOF/MS) method was adopted to detect the flavonoids, saponins, alkaloids, terpenoids in IM methanol extract. Data presented here is related to a published work Antioxidant and antibacterial activity of Ipomoea mauritiana Jacq.: A traditionally used medicinal plant in Bangladesh (Alam et al., 2020). Secondary metabolites were analyzed by the comparison of the mass fragmentation arrangements with Waters UNIFI library that enables for positive identification of the compounds based on the spectral match.

Aminoglycosides are a class of broad-spectrum antibiotics with several clinical uses. Owing to the ototoxicity and nephrotoxicity of aminoglycosides, therapeutic drug monitoring is required. This study aimed to devise a high-throughput method for identification and quantitative determination of aminoglycoside antibiotics in human plasma samples using ultra-performance liquid chromatography–quadrupole time-of-flight-mass spectrometry (UPLC–Q-ToF-MS). Plasma samples (100 µL) spiked with five aminoglycosides (streptomycin, spectinomycin, amikacin, kanamycin, and gentamycin) and an internal standard (ribostamycin) were diluted and centrifuged in aqueous formic acid and acetonitrile. The clear supernatant extract was evaporated and reconstituted in the mobile phase, of which 4 µL was subjected to UPLC–Q-ToF-MS. Prominent peaks were observed for the drugs within 3 min. The recoveries of five aminoglycosides from plasma samples were 92.6–120%. The regression equations showed excellent linearity (0.9999 ≥ r2 ≥ 0.9987) within the range of 1.0–100 µg/mL, and detection limits of 0.5–2.0 µg/mL. The coefficients of the intra- and inter-day variations for five drugs were less than 11.8%, while the accuracy of quantitation was in the range of 89–111%. In this study, a novel method was presented for identification and determination of aminoglycosides in human plasma samples using UPLC–Q-ToF-MS analysis. This method can be applied to high-throughput analysis used for clinical and environmental purposes.

Divya-Swasari-Vati (DSV) is a calcium-containing herbal medicine formulated for the symptomatic control of respiratory illnesses observed in the current COVID-19 pandemic. DSV is an Ayurvedic medicine used for the treatment of chronic cough and inflammation. The formulation has shown its pharmacological effects against SARS-CoV-2 induced inflammation in the humanized zebrafish model. The present inventive research aimed to establish comprehensive quality parameters of the DSV formulation using validated chromatographic analytical tools. Exhaustive identification of signature marker compounds present in the plant ingredients was carried out using ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC/QToF MS). This was followed by simultaneous estimation of selected marker components using rapid and reliable high-performance liquid chromatography (HPLC) analysis. Eleven marker components, namely gallic acid, protocatechuic acid, methyl gallate, ellagic acid, coumarin, cinnamic acid, glycyrrhizin, eugenol, 6-gingerol, piperine and glabridin, were selected out of seventy-four identified makers for the quantitative analysis in DSV formulation. Validation of the HPLC method was evaluated by its linearity, precision, and accuracy tests as per the International Council of Harmonization (ICH) guidelines. Calibration curves for the eleven marker compounds showed good linear regression (r2 &gt, 0.999). The relative standard deviation (RSD) value of intraday and interday precision tests were within the prescribed limits. The accuracy test results ranged from 92.75% to 100.13%. Thus, the present inclusive approach is first of its kind employing multi-chromatographic platforms for identification and quantification of the marker components in DSV, which could be applied for routine standardization of DSV and other related formulations.

Traditional Chinese medicines (TCMs) have been considered as important alternative therapeutics because of their significant medicinal benefits in specific diseases. Chinese herb formula is characterized by a vast molecule that differs in routine medicines. Due to TCMs chemical complexity, proper quality control has been a great challenge. Choosing the appropriate method to identify and qualify these compounds is an important work to ensure its safety, efficacy and quality control. Thus, this study aimed at providing novel information on high-resolution LTQ-Orbitrap mass spectrometer (UPLC-LTQ-Orbitrap-MSn) based identification of Bu Shen Yi Sui capsule (BSYSC), which is used in treating multiple sclerosis as a kind of TCMs. Under the proposed chromatographic conditions, 80 chemical components classified as anthraquinone, phenolic acid and phenylethanoid glycosides were separated and identified from BSYSC. Coupled with the high-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS/MS) method, eight of them were regarded as marker compounds for the quantitative evaluation of BSYSC. The identification and quantification with precision of UPLC-LTQ-Orbitrap-MSn and UPLC-QTOF-MS/MS could facilitate essential data for further pharmacokinetic studies of BSYSC.

The metabolism and pharmacokinetics of gefitinib (Iressa®, N-(3-chloro-4-fluorophenyl)-7-methoxy-6-(3-morpholino-propoxy)quinazolin-4-amine), a selective thymidylate kinase inhibitor for the epidermal growth factor receptor (EGFR), was studied after IV and PO administration to male C57BL6 mice at 10 and 50 mg/kg respectively.The pharmacokinetics and metabolism of gefitinib were investigated using a range of rapid UHPLC-MS and UHPLC-IM-HRMS methods, using both reversed-phase (RP) and hydrophilic interaction liquid chromatography (HILIC), to rapidly determine the drugs pharmacokinetics and metabolic fate.Rapid oral absorption resulted in peak plasma concentrations at 1 h of ca. 7 µg/mL, that declined with a half-life of 3.8 h (2.6 h for the IV route), and providing an estimated oral bioavailability of 53%. Gefitinib itself was the major circulating drug-related compound in plasma extracts, with a total of 11 metabolites identified.The urinary profiles determined using both HILIC and RP-UPLC-IM-MS detected gefitinib and 10 metabolites or 15 metabolites respectively including the detection of a number of novel glucuronide conjugates.Despite rapid, sub 5 min, LC profiling methods being employed metabolite coverage was shown to be high and compared well with that of previous studies. The metabolism and pharmacokinetics of gefitinib (Iressa®, N-(3-chloro-4-fluorophenyl)-7-methoxy-6-(3-morpholino-propoxy)quinazolin-4-amine), a selective thymidylate kinase inhibitor for the epidermal growth factor receptor (EGFR), was studied after IV and PO administration to male C57BL6 mice at 10 and 50 mg/kg respectively. The pharmacokinetics and metabolism of gefitinib were investigated using a range of rapid UHPLC-MS and UHPLC-IM-HRMS methods, using both reversed-phase (RP) and hydrophilic interaction liquid chromatography (HILIC), to rapidly determine the drugs pharmacokinetics and metabolic fate. Rapid oral absorption resulted in peak plasma concentrations at 1 h of ca. 7 µg/mL, that declined with a half-life of 3.8 h (2.6 h for the IV route), and providing an estimated oral bioavailability of 53%. Gefitinib itself was the major circulating drug-related compound in plasma extracts, with a total of 11 metabolites identified. The urinary profiles determined using both HILIC and RP-UPLC-IM-MS detected gefitinib and 10 metabolites or 15 metabolites respectively including the detection of a number of novel glucuronide conjugates. Despite rapid, sub 5 min, LC profiling methods being employed metabolite coverage was shown to be high and compared well with that of previous studies.

Radix Gentianae Macrophyllae (RGM) is a traditional Chinese medicine belonging to the Gentiana genus and including four species of herbs. Owing to the lack of characteristic constituents, it is difficult to discriminate RGMs of different origins or even differentiate between herbs in the same genus. The current research aimed to explore the characteristic aromatic compounds, verify their significance in distinguishing different origins of RGM herbs and provide a simple and effective quality evaluation method. A selective extraction method was developed for noniridoid compounds and the extract was then subjected to UPLC-QTOF-MS analysis to obtain the RGM-MS ion pair database for noniridoid components. An HPLC-DAD quantitative analysis method was further developed based on characteristic aromatic compounds (2-phenylethyl β-d-glucopyranoside, 2-methoxyanofinic acid and gentioxepine) after the ion screening in the MS database. By means of principal component analysis and hierarchical clustering analysis analysis, the significant relationship between aromatic compounds contents and different species of RGM was revealed. As a result, the significance of 2-phenylethyl β-d-glucopyranoside, 2-methoxyanofinic acid and gentioxepine in distinguishing four species of RGM herbs was verified and a sensitive and reproducible HPLC-DAD method was established using these markers, which can be used for the classification and quantitative analysis of RGMs.

Dioscorea polystachya, named Chinese yam, is widely cultivated as a functional food and natural medicine in China. There is currently little information about the chemical characteristics of Dioscorea polystachya in different organs (tuber cortex and tuber flesh) and at various ages. In this study, an ultra-high-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UPLC-QTOF/MS) was used to profile chemical compounds in Dioscorea polystachya. As a result, thirty-eight compounds were detected in yam tuber cortex and tuber flesh. More compounds were detected in yam tuber cortex than in tuber flesh. Compounds such as dehydroepiandrosterone, allantoin and flavonoids were selected as biomarker candidates. Dehydroepiandrosterone was found more abundant in tuber flesh, while allantoin and flavonoids showed higher levels in tuber cortex. Furthermore, the levels of dioscin, malvalic acid and sucrose differed significantly among age groups and were highest in the tubers at 2 years. While the levels of allantoin, adenosine and glutamine increased with the growing years and were highest at 4 years. Thus, 2-year old Dioscorea polystachya tubers could be harvested to prepare dioscin, malvalic acid and sucrose supplements. The 4-year-old Dioscorea polystachya tubers would be the best choice for obtaining a large amount of allantoin and adenosine in industrial production.

An original way of brewing Cyclocarya paliurus leaves, especially in China, is to steep leaves in hot water before people drink it directly. Recently, infusing tea leaves with cold water, a creative way in Taiwan, has become a popular way of making tea. This study was designed to investigate the differences in metabolites among three brewing methods (cold-brewing, steep-brewing, and boil-brewing) based on UPLC-QTOF-MS metabolomics experiments and the feasibility of cold-brewing methods for C. paliurus leaves. Unsupervised analysis (PCA) explained 54.6% (positive ion mode) and 57.4% (negative ion mode) of the total variance, whereas supervised analysis (OPLS-DA) with cross-validated R2Y and Q2 values > 0.5, could reveal potential metabolites with better discrimination among the three brewing methods. Fifteen potential differential metabolites were chosen and identified, and nine of them were further confirmed with reference standards. This study suggested that the cold-brewing method without an increase in temperature protected the phenol aromatic ring, thereby obtaining more phenolic acid compounds from C. paliurus leaves. These results provided a basis for making cold tea and promoting the development of cold tea with C. paliurus leaves as raw materials.

Cyperus has been commonly used as a multi-use medicinal plant in folk medicine worldwide. The objectives of our study were to determine the different metabolites in the Cyperus conglomeratus Rottb. methanol extract, and to assess its in vivo gastroprotective effect in ethanol-induced gastric ulcer model in rats. Serum levels of galactin-3 and TNF-&alpha, were employed as biochemical markers. To pinpoint for active agents, comprehensive metabolites profiling of extract via UPLC-qTOF-MS/MS was employed. A total of 77 chromatographic peaks were detected, of which 70 were annotated. The detected metabolites were categorized into phenolic acids and their derivatives, flavonoids, stilbenes, aurones, quinones, terpenes, and steroids. Rats were divided into six groups, healthy control, ulcer control, standard drug group, and 25, 50, 100 mg/kg of C. conglomeratus treated rats. Pre-treatment with C. conglomeratus alcohol extract significantly reduced galactin-3, and TNF-&alpha, in ethanol-induced ulcer model at 25, 50, and 100 mg/kg. Further histopathological and histochemical studies revealed moderate erosion of superficial epithelium, few infiltrated inflammatory cells, and depletion of gastric tissue glycoprotein in the ulcer group. Treatment with the extract protected the gastric epithelial cells in a dose-dependent manner. It could be concluded that C. conglomeratus extract provides significant gastroprotective activity in ethanol-induced gastric ulcer and ought to be included in nutraceuticals in the future for ulcer treatment.

Background Zhi-Zi-Da-Huang decoction (ZZDHD) is a famous Traditional Chinese Medicine decoction due to its therapeutic effects on clinical hepatobiliary disorders. ZZDHD is composed of Gardeniae Fructus, Rhei Radix et Rhizoma, Fructus Aurantii Immaturus, and Sojae Semen Praeparatum. With the development of current technology, dispensing granules have been widely used for convenience. However, limited research has been conducted to determine differences in the chemical compounds between dispensing granules and traditional decoction. Methods A strategy based on UPLC-qTOF-MS/MS and UPLC-DAD was established to quantitatively and qualitatively analyze the chemical compounds present in single- and co-boiled ZZDHD. First, we utilized UPLC-qTOF-MS/MS to identify the compounds in single- and co-boiled ZZDHD. Then, 15 compounds were quantitatively analyzed in ZZDHD by UPLC-DAD. Finally, fingerprint and chemometric analyses were adopted to evaluate the difference between single- and co-boiled ZZDHD. Results One hundred and forty-seven compounds were authenticated or determined according to their retention behaviors, mass mensuration, and characteristic fragment ions. In addition, 15 analytes of single- and co-boiled ZZDHD indicated a significant difference in the content of many compounds, including geniposide (G2), emodin, chrysophanol, daidzin, and crocin-I. The similarities of single and co-boiled ZZDHD were higher than 0.99, as evaluated by fingerprinting; 30 common peaks were evaluated by the chemometric analysis, which found 13 important variable values (VIP > 1) including C3, A3, crocetin, daidzin, C5, physcion, G2, genipin-1-O-β-D-gentiobioside (G1), chrysophanol, emodin, A2, A5, and C6. Conclusions This study provided an experimental basis for explaining the rationality of single-and co-boiled ZZDHD, and a study model for comparing the chemical substances between traditional decoctions and dispensing granules.

Data analysis during UPLC-MS non-targeted metabolomics introduces variation as different manufacturers use specific algorithms for data treatment and this makes untargeted metabolomics an application for the discovery of new biomarkers with low confidence in the reproducibility of the results under the use of different metabolomics platforms. This study compared the ability of two platforms (Agilent UPLC-ESI-QTOF-MS and Waters UPLC-IMS-QTOF-MS) to identify biomarkers in butterhead and romaine lettuce cultivars. Two case studies by different metabolomics platforms: (1) Waters and Agilent datasets processed by the same data pre-processing software (Progenesis QI), and (2) Datasets processed by different data pre-processing software. A higher number of candidate biomarkers shared between sample groups in case 2 (101) than in case 1 (26) was found. Thirteen metabolites were common to both cases. Romaine lettuce was characterised by phenolic compounds including flavonoids, hydroxycinnamate derivatives, and 9-undecenal, while Butterhead showed sesquiterpene lactones and xanthosine. This study demonstrates that high percentages of the most discriminatory entities can be obtained by using the manufacturers’ embedded pre-processing software and following the recommended processing data guidelines using commercial software to normalise the data matrix.

Background HuaTanJiangQi (HTJQ) is a classical Chinese medicine compound preparation, mainly used for clinically treating and improving chronic obstructive pulmonary disease (COPD) in China. Objective To establish a rapid and efficient analytical method for the identification and characterization of chemical constituents in HTJQ based on ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS). Method UPLC-QTOF-MS was used to rapidly separate and identify the chemical constituents of HTJQ via a gradient elution system. The accurate mass data of the protonated and deprotonated molecules and fragment ions were detected in positive and negative ion modes. Compounds of HTJQ can be identified and assigned by analyzing accurate mass measurements and ion fragmentation mechanisms and comparing them with a chemical compositions database. Results A total of 61 compounds in HTJQ were separated and identified, including 14 flavonoids, 16 organic acids, four isothiocyanic acids, eight butyl phthalides, two alkaloids, 10 terpenoids, four methoxyphenols and furanocoumarins, and three other compounds. The chemical compounds of HTJQ were identified and elucidated comprehensively for the first time. Conclusions A rapid, accurate, and efficient UPLC-QTOF-MS method has been developed for the identification of chemical components and applied to simultaneously evaluate the quality and effectiveness of HTJQ. Highlights Systematic identification of chemical constituents in HTJQ can provide a scientific and reasonable basis for the application of HTJQ in the clinical treatment of COPD.

OBJECTIVES: The study aim was to identify bioactive compounds in mango leaf tea using a new method - UPLC/Q-TOF-MS. Mango leaf tea is a natural product being investigated to manage type 2 diabetes due to its phytochemical properties. METHODS: Mango tea was extracted using 80% methanol overnight. The extract was analyzed with ultra-high-performance liquid chromatography-quadrupole time-of-flight (UPLC-Q-TOF) MS system (Waters Corp., Milford, MA) and injected into an Acquity UPLC BEH C18 column (2.1 mm × 100 mm, 1.7 µm, Waters Corp.). The column was equilibrated with distilled water containing 0.1% formic acid (FA) and eluted by a linear gradient of acetonitrile (ACN) containing 0.1% FA at a flow rate of 0.35 mL/min for 10 min and 40 °C of column temperature. RESULTS: The eluents were analyzed by A Vion IMS Q-TOF MS (Waters Corp.) with positive and negative electrospray ionization (ESI). The scan range of TOF MS data was 50–1500 m/z, the scan time was 0.2 sec, and the capillary and sampling cone voltages were 3 kV and 40 V, respectively. The desolvation flow rate and temperature were 800 L/h and 400 °C, respectively, and the source temperature was 100 °C. Leucine-enkephalin ([M + H] = 556.2771 Da; [M-H] = 554.2615 Da), used as a lack mass, was infused at a flow rate of 0.35 μL/min and a frequency of 10 s to ensure mass measurement accuracy of the metabolites analyzed by the instrument. Mass spectral data were collected from m/z 50 to 1500 with a scan time of 0.2 s. Collision energy was ramped from 10 to 40 eV for the collection of MS/MS data. The metabolites Mangiferin, quercetin/isoquercetin and iriflophenone 3-beta-glucoside were identified using ChemSpider in negative mode while only mangiferin and quercetin were defined in positive mode with different intensites: Mangiferin (421.07), quercetin/isoquercetin (303.05) and irrflophenone 3- beta- glucoside (407.097) that confirmed their molar mass. CONCLUSIONS: The UPLC/Q-TOF-MS technique is a practical and novel method for identifying the fragmentation pattern of metabolites in mango leaf tea by measuring accurate mass with excellent resolution and sensitivity. FUNDING SOURCES: N/A.