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Objective: Compound traditional Chinese medicine (CTCM) with the application of compatibility from multiple active ingredients with multiple-specific targets can achieve a synergistic effect on cancer therapy. This study is aimed to observe the compatibility effects of Aidi injection on the treatment of hepatocellular carcinoma and to explore the mechanism of CTCM. Methods: Aidi injection is a clinical compound prescription containing Mylabris, Ginseng, Astragalus, and Acanthopanax, which can inhibit tumor growth and induce apoptosis. In this study, the anticancer activity of Aidi injection, as well as its disassembled and combined compositions, had been evaluated by varying levels of polyamine biomarkers on human hepatoma Hep-G2 cells detected using ultrahigh-performance liquid chromatography-tandem mass spectrometry. Results: According to the different variations in polyamine levels, it was revealed that Mylabris and Ginseng had an antitumor effect, while Astragalus acted as an assistant and Acanthopanax had weak anticancer activity. The increased level of polyamines in Hep-G2 cells had been found in HL-7702 cells. On combining Mylabris and Ginseng, polyamine levels went close to the normal level, which was even more marked when Astragalus was added. Aidi injection acted like the combination of Mylabris, Ginseng, and Astragalus. Conclusions: This study established a quantitative evaluation of the compatibility effects of Aidi injection based on polyamine biomarkers and evaluated the consistency of its anticancer effect, providing a manner to research the efficacy evaluation of CTCM. Moreover, the correlation between polyamine metabolism and anticancer activity can be used in anticancer drug screening.

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Objective: Gegen Qinlian decoction (GQD) is a classical traditional Chinese medicine formulation which has been used for almost 2000 years. At Guang'anmen Hospital, Beijing, a modified GQD version (mGQD) with seven instead of four herbal ingredients has been applied to treat Type 2 diabetes. Quality control is a crucial prerequisite for the therapeutic application of herbal medicines. For the identification of products derived from classical GQD, the Chinese Pharmacopeia requires the analysis of only three marker compounds. Because mGQD is a more complex mixture containing seven herbs and hundreds of constituents, the pharmacopoeia method for GQD is inadequate. Materials and Methods: A more comprehensive characterization of the formula's constituents has been developed using ultra-high-performance liquid chromatography-diode array detection (UHPLC-DAD)-Q-Exactive-mass spectrometry (MS) in electrospray ionization positive and negative mode. Moreover, a new method for the fingerprint analysis of mGQD via high-performance thin-layer chromatography (HPTLC) has been established. Results: Altogether, 91 compounds have been assigned to their originating plants and 84 substances were identified either by comparison with authentic references or with data from the literature. The HPTLC method is based on the application of two different mobile phases and is able to detect both lipophilic and hydrophilic constituents of mGQD. Conclusions: The modified GQD was extensively characterized by UHPLC combined with DAD and Q-Exactive Orbitrap high-resolution MS detection, leading to the assignment and identification of compounds present in the decoction. In addition, a new method for the fingerprint analysis of the mGQD using HPTLC was established, which allows fast and simple identification of the herbal ingredients in the mixture.

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Objective: Quality control of traditional Chinese medicine (TCM) begins with the chemical basis elucidation. The root of Stephania tetrandra has long been utilized as an antirheumatic, analgesic, and diuretic TCM, Stephaniae Tetrandrae Radix (STR; Fang-Ji). Powerful analytical strategies enabling its multicomponent characterization is still rare. Methods: A rapid, reliable, and enhanced profiling approach, by ultra-high performance liquid chromatography coupled with ion mobility/quadrupole time-of-flight mass spectrometry (UHPLC/IM-QTOF-MS) and automatic peak annotation facilitated by computational matching of in-house library, was established and utilized to characterize the multicomponents from STR. A knockout strategy was utilized by automated valve switching to overcome the interference of predominant peaks. Results: Good chromatographic separation was achieved within 17 min on a reversed-phase BEH C18 column eluted with acetonitrile/0.1% ammonium hydroxide in water, while data-independent high-definition MS^E (HDMS^E) in positive mode was applied to acquire the MS² data by using a VionTM IM-QTOF instrument, which in theory, could cover all the profiled precursor ions. An in-house library of 163 compounds was established and incorporated into the UNIFITM platform. By feat of these efforts, we were able to identify or tentatively characterize 76 alkaloids from the methanolic extract of STR, including 14 aporphine-type, four morphine-type, 48 bisbenzylisoquinoline-type, seven tetrahydroprotoberberine-type, one protopine-type, one benzylisoquinoline-type, and one other. Four-dimensional information, such as the retention time, collision cross section (CCS), high-accuracy MS1 and MS2 data, for each component was provided. Conclusions: The systematic multicomponent characterization of STR was accomplished with high coverage, high degree of automation, and high reliability.

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Objective: Small molecules in snow chrysanthemum such as flavonoids, phenolic compounds and amino acids have been extensively investigated. No study to date has focused on water-soluble oligosaccharides. The objective of this study is identification and determination of water-soluble oligosaccharides in snow chrysanthemum. Methods: The oligosaccharides in snow chrysanthemum were identified by high performance thin layer chromatography (HPTLC), liquid chromatography-mass spectrometry (LC-MS) combined MS library and methylation analysis for the first time. Subsequently the oligosaccharides were determined by high performance liquid chromatography with a charged aerosol detector (HPLC-CAD). Results: The oligosaccharides in snow chrysanthemum were identified as inulin-type fructooligosaccharides (FOS). The yield of FOS (DP3~DP13) in the first extraction was over 97.6%. The RSDs of repeatability in three sample amount levels (0.08 g, 0.1 g, 0.12 g) are lower than 4.8% and the RSDs of stability are less than 3.5%. The recoveries of FOS (DP3~13) were ranging from 96.9% to 105.6%. The contents of FOS (DP3~DP13) in flowers of snow chrysanthemum from different regions of China were greatly variant. Conclusion: This is the first time to identify and quantify FOS in snow chrysanthemum which is helpful for its performance in the in the fields of biomedical, agriculture and functional food industry as well as development of the quality control methods. In addition, the identification approach developed in this work can also be used for screening potential natural sources containing FOS..

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Objective: There are different geographic origins of Aconiti Kusnezoffii Radixs (AKRs) sold in the market with different quality. This study aims to establish a rapid analysis method to distinguish the different geographic origins of AKRs and to realize the rapid evaluation of their quality. Methods: An ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC-Q-TOF MS) method was utilized to acquire the constituents' information of AKRs from different geographic origins. MS^E data and Progenesis QI software were employed to identify the chemical constitutes. Principal component analysis (PCA) was applied to comparing MS data to find the chemical markers of AKRs from different geographic origins. Results: Twenty-three components were detected and 17 out of them were identified, including diester-diterpenoid alkaloids, monoester-diterpenoid alkaloids , and amine-diterpenoid alkaloids. Three pairs of isomers were detected and two of them were distinguished by the retention time of standard samples. Thirteen chemical markers were screened out through PCA and orthogonal partial least square discriminant analysis. Through detecting Napelline or isomer of Napelline (m/z 360.2530) and Aconifine (m/z 662.3170), AKRs from inner Mongolia autonomous could be screened. According to the existence of benzoylaconine (m/z 604.3108) and Indaconitine (m/z 630.3159), it could be confirmed that the AKRs are from Xinjiang Uygur autonomous. AKRs that cannot detect compounds above-mentioned could be from Liaoning or Shanxi Province. Conclusions: The chemical profile could be used not only to distinguish the AKRs from different geographic origins but also to identify the true and false of AKRs. This study lays a foundation for the study of efficacy and toxic of AKRs.

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Objective: Ginkgo biloba leaves, as an herbal medicine or dietary supplement, have been widely used worldwide. In this study, an integrated analytical method was established for the comprehensive analysis of flavonoids in G. biloba leaves. Materials and Methods: A practical chromatographic method combining high-performance liquid chromatography fingerprint analysis and quantitation was used to simultaneously determine 11 flavonoids (6 flavonol glycosides and 5 biflavones) in G. biloba leaves from different regions. Results: A total of 11 characteristic peaks were identified accurately, and the similarity of fingerprints ranged from 0.944 to 0.996. Methodology validation revealed appropriate linearity ( R² ≥ 0.9997), precision, repeatability, stability, and recovery. The total contents of the six flavonol glycosides and five biflavones were within the range of 2.142-8.378 mg/g and 3.759-5.675 mg/g in 19 batches of samples, respectively. Among them, two coumaroyl flavonol glycosides were the predominant components. Conclusions: In this study, a convenient and reliable approach was successfully employed for the comprehensive evaluation of flavonoids in G. biloba leaves, which also provided a reference for its quality standard.

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Objective: In this study, a comprehensive and effective quality method for evaluating the efficacy of ShuXueNing injection (SXNI) was developed. Materials and Methods: Quantitative high-performance liquid chromatography fingerprint, the quantitative analysis of multicomponents by a single marker (QAMS) method, hierarchical cluster analysis (HCA), and orthogonal partial least squares discrimination analysis (OPLS-DA) were used to distinguish 53 batches of SXNI samples from 7 manufacturers. Results: A total of 53 batches of samples were analyzed to establish antithesis fingerprint of SXNI, and 12 peaks of the common model were collected and used for the similarity analysis. Meanwhile, six index flavonoid components were determined by the QAMS method, using rutin as internal reference substance. The accuracy of the QAMS method was confirmed by investigating the relative deviation between the QAMS method and the traditional external standard method. The results demonstrated that there was no significant difference (RE < 1%), suggesting that QAMS was a reliable and convenient method for the content determination of multiple components. The HCA and OPLS-DA methods drew a similar conclusion. The 53 batches of SXNI samples from 7 manufacturers were categorized into five groups, indicating that chemometrics could reveal the quality differences of SXNI between the manufacturers. Conclusions: The method established herein was efficient and successful in assessing the quality of SXNI, and that it may be potentially employed in the quality control of related products composed of Ginkgo biloba extract.

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Objective: Belamcandae Rhizoma and Iridis Tectori Rhizoma are easily confused with each other. The main objective of this study is to distinguish them using chemical analysis. Materials and Methods: Thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC) fingerprint methods were established to compare the chemical profile, while HPLC quantitation was used to determine the contents of three isoflavones in thirty batches of Belamcandae Rhizoma and Iridis Tectori Rhizoma samples. Results: The two herbs could be distinguished by TLC using acetic acid- n hexane-ethyl acetate (1:90:80 v/v/v) as the mobile phase, according to the fluorescent band under 366 nm at R_f 0.2. In total, 12 compounds were identified in the 24-min HPLC fingerprint. The similarity coefficient between the two herbs was 0.54 ± 0.01. Mangiferin (1), tectoridin (2), iridin (3), irigenin (5), irisflorentin (6), and iristectorin A (9) were the main peaks in Belamcandae Rhizoma, while tectoridin (2) and tectorigenin (4) were the major peaks in Iridis Tectori Rhizoma. The contents of 2 in Iridis Tectori Rhizoma (2.50 ± 0.20 %) were 8.93 times higher than that of Belamcandae Rhizoma (0.28 ± 0.08 %), while the ones of 5 and 6 were slightly lower in Iridis Tectori Rhizoma. Conclusions: The study established fast and effective methods to distinguish Belamcandae Rhizoma from Iridis Tectori Rhizoma.

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Objective: Authentication is vital to the reduction of the misuse of Panax species due to their extensive array of uses and similarities between species. However, the current authentication approach is time-consuming, laborious, and costly. The aim of this study is to discriminate the botanical origins of five species in Panax genus by a rapid and simple approach. Methods: Here, an electronic tongue (E-tongue) was applied to discriminate the botanical origins of five species of Panax, i.e., Panax quinquefolius, Panax japonicus, P. japonicus var. major, Panax zingiberensis, and Panax notoginseng (representative high-, middle-, and low-latitude plants), and the four geographical origins of P.japonicus and P. japonicus var. major plants. Data preprocessing methods, including principal component analysis (PCA), hierarchical cluster analysis (HCA), and linear discriminant analysis (LDA), were used. Results: Three models can discriminate five species of Panax genus and four plants of P. japonicus and P. japonicus var. major from different geographical origins. LDA was superior to PCA and HCA in terms of satisfactory classification. Conclusion: The findings confirmed the potential of the E-tongue for performing rapid, simple, and cost-effective discrimination via LDA.

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Objective: To develop a reversed-phase high-performance liquid chromatography method for the quantification of major ginsenosides in red ginseng (RG, the steamed and dried root of the cultivar of Panax ginseng C. A. Mey). Methods: A feasible method was developed in strict accordance with chromatographic properties of eight ginsenosides. Their contents could be unveiled with conventional external standard method, or as an alternative, using ginsenoside Rg1 as the single reference standard by means of seven conversion factors. Those parameters had been validated on different chromatographic columns and instruments. Results: Twenty-one batches of RG samples were determined. In addition, the chromatograms of RG and confusing species, including Panax ginseng, Panax quinquefolium, and Panax notoginseng, were apparently different. Conclusions: The method was proved to be efficient for the quality control of RG.

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Background: Chinese Danggui (Angelica sinensis) and Japanese Danggui (Angelica acutiloba) are evaluated as the same in using and critical of quality control in Vietnamese Pharmacopoeia. In Vietnam, Japanese Danggui were acclimatized and cultivated in several regions in recent years. Despite the huge climatic difference between Vietnam and Japan, Japanese Danggui grows very well in Vietnam. However, there are no studies to assess the overall quality of this medicinal herbs. Aims and Objectives: The aim of this study is to develop a method to identify and assay simultaneously 5 component compounds of these crude herbs: chlorogenic acid, ferulic acid, scopoletin, xanthotoxin and ligustilide by high-performance liquid chromatography with photodiode array detector (HPLC-PDA). Materials and Methods: The procedure was optimized by using column Phenomenex Gemini 5 μm PR C18, 15 x 4,6 mm with the detection wavelength set at 321 nm for detector PDA and mobile phase was composed of (A) ACN and (B) aqueous solution 1% of acid acetic using a gradient elution. Analytes were performed at 30°C with a flow rate of 1.0 mL/min. Results: The developped method were fully validated for linearity, accuracy, recovery and met the validation requirements, proved practical applicability for the quality control of these herbs and related products. Conclusion: The method was successfully applied to the quantification of five markers simultaneously from collected samples.

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Objective: Chuanxiong Rhizoma (CR, the dried rhizomes of Ligusticum chuanxiong) is a well-known traditional Chinese medicine that promotes qi to activate blood, dispels wind, and relieves pain. To date, more than 118 constituents of CR have been isolated and identified. However, the in vivo mechanism of CR decoction is unclear and needs further investigation. In addition, to clarify the effective forms of CR, it is essential to reveal the absorbed constituents and metabolites of CR. Materials and Methods: The absorbed constituents and metabolites in urine and plasma samples of rats orally administered with CR decoction were screened and characterized using a high-performance liquid chromatography with diode array detector and combined with electrospray ionization ion trap time-of-flight multistage mass spectrometry technique. Results: In total, 102 compounds, including 11 absorbed constituents (eight phthalides and three phthalic acids) and 91 metabolites (71 phthalide-related and 20 phenolic acid-related), were detected in drug-containing rat urine and plasma samples, among which 33 were new metabolites of either CR or its constituents. Based on the structures of these metabolites, six phthalides (ligustilide, senkyunolide I/H, senkyunolide J/N, and butylidenephthalide) and three phenolic acids (ferulic acid, isoferulic acid, and caffeic acid) were proposed as their precursors. They were also deduced to be the main absorbed constituents of CR decoction, which should have closer relationships with its pharmacological effects than other constituents. Phthalide-related metabolites were formed through the metabolic reactions of hydration, hydroxylation, cysteine conjugation, acetylcysteine conjugation, methanethiol conjugation, mercaptomethanol conjugation, glucuronidation, and sulfation, whereas the phenolic acid-related metabolites were mainly formed by glucuronidation and sulfation. Conclusions: Six phthalides and three phenolic acids were shown to be the main precursors of the metabolites of CR, and 33 compounds were new metabolites of either CR or its constituents. These results are helpful for further understanding of the in vivo mechanism and effective forms of CR.

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Objective: The objective of the study was to develop a rapid and sensitive ultra-performance liquid chromatography-tandem mass spectrometric method for the determination of tetrandrine, fangchinoline, and cyclanoline in rat plasma and to investigate their pharmacokinetics after oral administration of Stephaniae Tetrandrae Radix extracts. Methods: Sample pretreatment involved methanol pretreatment and liquid–liquid extraction of ethyl acetate from plasma with methanol. Tramadol was used as the internal standard. The analysis was performed using an high strength silica T3 column (100 mm × 2.1 mm, 1.8 μm) and a gradient elution method consisting of mobile phase solution A (0.1% formic acid in water) and B (acetonitrile) at a flow rate of 0.4 mL/min. The detection was performed using a triple quadrupole tandem mass spectrometer in the multiple reaction monitoring mode and using an electrospray ionization source in the positive ionization mode. Results: High efficiency was achieved with an analysis time of 4 min/sample. The calibration curve linear in the concentration range of 1250 ng/ml ( R² ≥ 0.9900) and the lower limit of quantification is 1 ng/ml. The intraday and interday precision (relative standard deviation) values were lower than 9.4. Accuracy (relative error) was within 10.3% at all three quality control levels. Conclusions: This method was successfully applied in pharmacokinetics of tetrandrine, fangchinoline, and cyclanoline in rats after oral administration of Stephaniae Tetrandrae Radix extracts. The maximum plasma concentration ( C_max) of tetrandrine, fangchinoline, and cyclanoline was 124.71 ± 16.08, 84.56 ± 3.28, and 57.61 ± 6.26 ng/mL, respectively. The time to reach C_max was 10.39 ± 3.04 for tetrandrine, 10.17 ± 3.04 for fangchinoline, and 6.40 ± 3.16 for cyclanoline. The pharmacokinetic results might help further guide the clinical application of Stephaniae Tetrandrae Radix.

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Objectives: A rapid and sensitive gas chromatography–mass spectrometry (GC–MS) method for quantitative and qualitative analysis of essential oil from Curcuma wenyujin rhizomes was established. Methods: The essential oil of C. wenyujin rhizomes was extracted by supercritical CO2 extraction (SFE). Six main bioactive compounds (eucalyptol, β-elemene, curzerene, germacrone, curdione, and curcumol) were analyzed in selected ion monitoring mode (SIM). Results: Curzerene is not originally present in C. wenyujin rhizomes, but is a product of the transformation of furanodiene at high temperature. The six target components demonstrated good linearity (R2 > 0.9979) over a relatively wide concentration range. The interday and intraday variations had relative standard deviation values less than 5% and the average recovery ranged from 96.95% to 100.04%. The limit of quantitation ranged from 0.032 to 0.235 μg/mL. The developed method was successfully used to analyze the six compounds in 17 samples collected from different origins. Significant variation was observed for the concentrations of the six compounds. In addition, 51 constituents were identified in C. wenyujin rhizome essential oil, consisting of 87.66% of the total essential oil, including curdione, curzerene, dehydrocurdione, germacrone, 1,4-bis(2-benzimidazoyl)benzene, neocurdione, curcumenone, and β-elemene. Conclusions: The proposed method will be useful in the quality control of C. wenyujin rhizome essential oil production.

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Objective: The study objective was to determine phenolic components for the quality control (QC) of cultivated Sarcandra glabra (Thunb.) Makino ( S. glabra). Materials and Methods: A sensitive, ultra-high-performance liquid chromatography-tandem mass spectrometric method for the simultaneous determination of 12 phenolic components has been developed. Six caffeoylquinic acids, two caffeoylshikimic acids, and four flavanonol glucosides were selected for the comprehensive analysis of distribution in different parts (root, stem, and leaf). Results: Twelve phenolic components were linear in the concentration range of 0.005–5.0 μg/mL ( R² > 0.995). The relative standard deviation of intra-day and inter-day precision across three validation runs over the entire concentration range was <5%. The recovery determined was within 5% in terms of relative error. Our results showed that the 12 phenolic compounds were mainly distributed in leaves and stems far more than those in roots. Conclusions: This study provided an ultra-high-performance liquid chromatograph with triple-quadrupole mass spectrometer quantitative method of 12 phenolic components for the QC of cultivated S. glabra. It was found that the phenolic components were significantly accumulated in the aerial parts (stems and leaves) of cultivated S. glabra.

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Objectives: An enzyme-linked immunosorbent assay (ELISA) and colloidal gold-based immunochromatographic (ICG) strip assay will be developed for the rapid and high-throughput detection of atrazine (ATZ) in medicinal herbs. Methods: A monoclonal antibody against ATZ was obtained after the immunization of mice, cell fusion, and hybridoma screening, and the antibody was used to develop direct competitive ELISA (dcELISA) and the ICG strip assay. Results: Both dcELISA and ICG strip methods were established, optimized, and validated for the detection of ATZ in Salviae miltiorrhizae radix et rhizome, Astragali radix, and Isatidis radix. dcELISA had a half-maximum inhibition concentration of 10.56 ng/mL (Salviae miltiorrhizae radix et rhizome), 7.6 ng/mL (Astragali radix), and 8.15 ng/mL (Isatidis radix). The limit of detection (LOD) of the ICG strip assay was 12.5 ng/mL (Salviae miltiorrhizae radix et rhizome), 12.5 ng/mL (Astragali radix), and 6.25 ng/mL (Isatidis radix) in different herb matrices. Due to the recognition characteristics of the monoclonal antibody for the pesticides ATZ, propazine, sebuthylazine, and prometryn, the detection results of real samples by the two immunoassays were confirmed by liquid chromatography–tandem mass spectrometry, which proved the accuracy and reliability of the established methods. Conclusion: The proposed dcELISA and ICG strip methods were suitable for the rapid, convenient, and high-throughput detection of ATZ in these medicinal herbs.

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