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MOLECULES · 2018 ·Vol. 23 ·期 8 ·2045 · IF 3.098

A Comprehensive Quality Evaluation Method Based on C30-HPLC and an Analytic Hierarchy Process for the Chinese Herbal Formula, Erzhiwan

Ying Nie,Weifeng Yao

The quantitative analysis of multiple indexes remains an important quality evaluation method of traditional Chinese medicine (TCM) herbal formulas. The Chinese Pharmacopoeia 2015 only stipulates the content of a single component, specnuezhenide, in Erzhiwan composed of the Fructus Ligustri Lucidi (FLL) powder and aqueous extracts of Herba Ecliptae (HE). To generalize the intrinsic quality of Erzhiwan, a novel C30-HPLC method with good precision, accuracy, and reproducibility was developed for the simultaneous determination of six compounds, including two isomers, and then an analytic hierarchy process was further applied to integrate and discriminate the quality of four samples prepared via different methods. The results of the analysis were in agreement with the antioxidant tests in vitro. This comprehensive strategy could provide a reference and suggestions for the improvement of the quality evaluation method of TCM herbal formulas.Keywords:analytic hierarchy process;C30-HPLC;Erzhiwan;herbal formula;quality evaluation

CAS / MDL: 7664-38-2
研究领域: 中药学 · 分析化学
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JOURNAL OF FOOD SCIENCE · 2021 ·Vol. 86 ·期 11 ·4828-4839 · IF 3.167

Simultaneous analysis of 20 free amino acids by a single marker combined with an HPLC fingerprint evaluation of Dendrobium huoshanense

Jing-wen Hao,An-ling Zhu,Nai-Dong Chen,Xiao-quan Liu,Qiang Li,Hui-min Xu,Wei-Han Yang,Chao-feng Qin,Jin-Dong Wu

A phenylhexyl isothiocyanate (PITC) precolumn derivatization quantitative analysis of multicomponents by a single marker (QAMS) strategy for the simultaneous analysis of 20 free amino acids (FAA) in Dendrobium huoshanense is proposed. The method was validated by the linearity, limit of detection (LDO), and limit of quantitation (LOQ), recovery, precision, and stability. The results showed that when applying the established method, the LOQ of the FFAs was lower than 1 ng/ml except threonine (1.32 ng) and cysteine (1.16 ng). The QAMS investigation revealed that, using any one of the 20 FAAs as the reference internal standard, no significant differences were observed between the external standard method and the QAMS method for the quantification of FAAs in D. huoshanense by PITC precolumn derivatization [The relative standard deviation (RSD, %) by QAMS and ESM were all below 5%]. HPLC fingerprint investigation combined with similar analysis (the similarity values for S1–S25 were >0.875) and quality fluctuation analysis showed that the cultivation environment might have a great effect on the accumulation of FAAs in D. huoshanense . Overall, our study showed that we might increase the accuracy and scope of the simultaneous quantification of multicomponents using the QAMS technique by being derivatized with a strong UV absorbing group, and QAMS combined with chromatographic fingerprinting can be considered good quality criteria for the quality control of D. huoshanense and may provide analytical technical support for research on Maillard Reaction during the further processing of D. huoshanense .

研究领域: 药用植物学 · 分析化学
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2024 · IF 4

Fermentation-linked conversion of dimethylpyrazines in moutai-flavor liquor: Insight from HPLC-FLD analysis

Hui Xu,Zhizhi Yang,Baote Huang,Peng Meng,Shuling Huang,Jicheng Chen

Moutai-flavor Baijiu (MFB), is renowned worldwide for its mysterious brewing process and its sauce-like flavor. Dimethylpyrazines (DMPs) are functional flavor compounds that make significant contributions to the aroma of MFB. To investigate the variation rule of DMPs during the brewing process of MFB, and to gain insights into the link between of DMPs and Moutai-flavor, we developed a simple, rapid, and effective HPLC-FLD method. The detection limits and quantification limits of our proposed method ranged from 0.008 to 0.035 mg/L, with an RSD of precision of less than 2 %. And the average recoveries ranged from 98 % to 100.48 %. The results showed that DMPs initially increased, reaching peak in 6th round with a concentration up to 14.997±0.414 mg/L, and then decreased during fermentation. In the aging stage, DMPs displayed a gradual upward trend, peaking at 10.052±0.252 mg/L after 7 years, before experiencing a minor decline at 9 years. These conversion behaviors are closely related to microbial metabolic activity and the Maillard reaction. We found high content of DMPs from the 4th-6th rounds (A round of fermentation takes a month) and the aged 7 years Baijiu have been described with strong sauce aroma and superior quality. This study provides a technical for focusing further investigating the unique flavor of Baijiu, revealing the conversion behavior of DMPs during the brewing process and their potential causes.

研究领域: 食品科学 · 微生物学 · 化学分析
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TALANTA · 2015 · IF 3.545

Indirect identification of antioxidants in Polygalae Radix through their reaction with 2,2-diphenyl-1-picrylhydrazyl and subsequent HPLC–ESI-Q-TOF-MS/MS

Qiyuan Shi,Jiale Chen,Qinfen Zhou,Houliang Lei,Lianjun Luan,Xuesong Liu,Yongjiang Wu

A rapid and efficient method for the identification of antioxidants in the traditional Chinese medicine Polygalae Radix (PR) by HPLC–ESI-Q-TOF-MS/MS is described. The method is based on the hypothesis that upon reaction of antioxidants with 1,1-diphenyl-2-picrylhydrazyl (DPPH), the peak areas of compounds with potential antioxidant activities in the HPLC chromatogram will be significantly reduced in comparison to the untreated sample. The identity confirmation was achieved by Q-TOF-MS/MS technique. With this method, eight components were proposed possessing potent antioxidant activity. They were identified as sibiricose A5, sibiricose A6, sucrose monoester, polygalaxanthone III, tenuifoliside B, 3',6-disinapoylsucrose (DISS), sucrose diester , tenuifoliside C, respectively. DISS was proposed to be the most potent one. The antioxidant activity of DISS was evaluated by DPPH, ABTS radical scavenging assay and ferric-reducing antioxidant power (FRAP) assay in vitro. Vitamin C (Vc) was used as positive control substance. DISS showed moderate DPPH (DISS's IC 50 value was 1024.17   μg/mL, Vc's was 294.68   μg/mL) and ABTS (IC 50 324.13   μg/mL, Vc's was 117.50   μg/mL) free radical scavenging capacity and ferric-reducing antioxidant power. DISS can be used as a new source of natural antioxidant in foods and cosmetics.

CAS / MDL: 28752-68-3
研究领域: 中药化学 · 分析化学 · 药理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2012 · IF 2.888

Simultaneous determination of gastrodin and puerarin in rat plasma by HPLC and the application to their interaction on pharmacokinetics

Li Jiang,Jundong Dai,Zhenlin Huang,Qinghua Du,Jiahao Lin,Yurong Wang

Gastrodin (Gas) and puerarin (Pur) are bioactive substances derived from traditional Chinese medicine Gastrodia elata and Radix Puerariae , respectively, which were often used together in Chinese clinical prescriptions. Their injections were used in combined way for treatment of some cardiocerebrovascular diseases in clinic, especially for vertigo due to vertebrobasilar ischemia. In this paper, interaction of gastrodin and puerarin in rat plasma pharmacokinetics via intragastic ( i.g. )/intravenous ( i.v. ) administration was investigated. A reliable HPLC method was developed for simultaneous determination of Gas and Pur in rat plasma with a linear range of 0.101–101   μg/mL for Gas and 0.0500–5.98   μg/mL for Pur ( r 2   >   0.993). The LLOQ, LOD of Gas and Pur were determined to be 0.101, 0.0486   μg/mL, and 0.05, 0.0245   μg/mL, respectively. The intra-day and inter-day precision were all less than 12.0%, whilst the accuracy were all within 96.4   ±   6.00%. The proposed method has been successfully applied to the pharmacokinetic study of the analytes in rats after i.g. / i.v. administration of Gas and Pur alone or combined with each other ( i.g. : 40   mg/kg Gas, 400   mg/kg Pur; i.v. : 20   mg/kg Gas, 20   mg/kg Pur). Blood samples were collected from retinal vein plexus of rats at predetermined time points and plasma containing the internal standard tyrosol (IS) were precipitated by methanol and chromatography was carried out on a C 18 column with a gradient mobile phase of ACN–H 2 O with 0.05% phosphoric acid as a modifier. The pharmacokinetic profiles of combined administration were found to be distinct from those of given alone. The C max , T max , T 1/2 , MRT of Gas administrated alone or combined with Pur via i.g. were 21.7   μg/mL, 0.250   h, 2.81   h, 0.830   h and 18.4   μg/mL, 0.550   h, 0.970   h, 1.37   h, respectively, of Pur administrated alone or combined with Gas via i.g. were 0.490   μg/mL, 1.95   h, 1.33   h, 2.10   h and 2.01   μg/mL, 0.570   h, 4.00   h, 5.10   h, respectively. The relative oral bioavailability of Pur in combined administration was 10.7 times as much as that of single administration, whilst 1.52 folds in Gas. These results indicate that co-administration of Gas and Pur is a promising combination to gain higher bioavailability and it is suggested that doctors pay more attention to the dosages of the two when simultaneously using both of them.

研究领域: 药理学 · 中药学
✓ 已验证 DOI PubMed 高影响因子
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Chinese Herbal Medicines · 2019 · IF 0

Monosaccharide analysis and fingerprinting identification of polysaccharides from Poria cocos and Polyporus umbellatus by HPLC combined with chemometrics methods

Jie Liu,Jing Zhou,Qian-qian Zhang,Min-hang Zhu,Mo-li Hua,Yun-hui Xu

Objective Poria cocos and Polyporus umbellatus are similar medicinal fungi in traditional Chinese medicines . A method for fingerprint analysis of monosaccharide composition of polysaccharides by HPLC combined with chemometrics methods has been developed for characterization and discrimination of them in this research. Methods The polysaccharides were extracted by decocting in water, and then completely hydrolyzed with hydrochloride. Monosaccharides in the hydrolyzates were derivatized with 1-phenyl-3-methyl-5-pyrazolone (PMP) for HPLC analysis. More than 20 batches of P. cocos and P. umbellatus from different regions were analyzed. Results The fingerprints of P. cocos showed five common characteristic peaks, which were identified by comparing with the reference substances. The five peaks corresponded to the derivatives of mannose , ribose , glucose, galactose , and fucose . At the same time, the fingerprints of P. umbellatus showed eight common characteristic peaks, of which seven were identified as the derivatives of mannose, ribose, rhamnose , glucose, galactose, xylose , and fucose. Moreover, the similarity of their fingerprints was respectively calculated by the Similarity Evaluation System for Chromatographic Fingerprint of TCM published by China Pharmacopoeia Committee (Version 2004A). And the data were further processed by hierarchical cluster analysis (HCA) and principal component analysis (PCA). The similarity evaluation and HCA indicated that there were no significant difference in P. cocos or P. umbellatus samples from different geographical regions, but PCA was performed to characterize the difference in monosaccharide constituents between P. cocos and P. umbellatus , and linear discriminant analysis (LDA) showed the overall correct classification rate was 100%. Conclusion The fingerprint analysis method of monosaccharide composition of water-soluble polysaccharides can distinguish P. cocos and P. umbellatus , and can be applied for the authentication or quality control for P. cocos and P. umbellatus.

CAS / MDL: 89-25-8
研究领域: 中药学 · 分析化学
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MICROCHIMICA ACTA · 2016 ·Vol. 183 ·期 8 ·2467-2472 · IF 4.831

Magnetic solid-phase extraction of triclosan using core-shell Fe3O4@MIL-100 magnetic nanoparticles, and its determination by HPLC with UV detection

Yang Yang,Ma Xiaowei,Feng Fan,Dang Xueping,Huang Jianlin,Chen Huaixia

The article describes the synthesis of core-shell magnetic nanoparticles (MNPs) of the type Fe 3 O 4 @MIL-100 (MIL standing for Material Institut Lavoisier), and their application as sorbent for magnetic solid-phase extraction (MSPE) of triclosan. The MNPs were prepared via circular self-assembly of ferric chloride and benzenetricarboxylic acid. The functionalized MNPs were characterized by transmission electron microscopy, FTIR and thermogravimetry. Following extraction, triclosan was eluted with ammoniacal methanol and then submitted to HPLC with UV detection. The amount of magnetic microspheres, sample pH and ionic strength, adsorption time, desorption time, desorption solvent and the volume of the eluent were optimized. Under optimum conditions, the method showed good linearity in the 0.1 to 50 mg·kg −1 triclosan concentration range in toothpaste samples. Other features include (a) intra-day and inter-day relative standard deviations (RSD, for n  = 4) of <5.5 %, (b) a 30 μg·kg −1 limit of detection, and (c) extraction recoveries between 90.86 % and 101.1 %. The method was successfully applied to the determination of triclosan in children’s toothpaste. The article describes the synthesis of core-shell magnetic nanoparticles (MNPs) of the type Fe 3 O 4 @MIL-100, and their application as sorbent for magnetic solid-phase extraction (MSPE) of triclosan.

研究领域: 分析化学 · 环境科学 · 材料科学
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RSC Advances · 2021 ·Vol. 11 ·期 48 ·30102-30108 · IF 3.361

Novel hydrophobic deep eutectic solvent for vortex-assisted liquid phase microextraction of common acaricides in fruit juice followed by HPLC-UV determination

Setareh Rostami-Javanroudi,Masoud Moradi,Kiomars Sharafi,Nazir Fattahi

In the present research, several novel and natural hydrophobic deep eutectic solvents (DESs) were prepared using methyltrioctylammonium chloride (MTOAC) as the hydrogen bond acceptor (HBA) and different types of straight chain alcohols as hydrogen bond donors (HBDs). One of the DESs composed of MTOAC and n-butanol was advantageously used to develop a vortex-assisted liquid phase microextraction (VALPME) method combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) for the determination of common acaricides in fruit juice samples. Several important parameters influencing extraction efficiency were investigated and optimized, including the type and volume of DES, sample solution pH, effect of salt addition and, extraction and vortex time. Under optimal experimental conditions, the method showed good linearity with the correlation coefficients (R2) of 0.9986–0.9991 in the linear range of 2–300 μg L−1, low limits of detection of 0.5–1 μg L−1 and acceptable extraction recoveries in the range of 85–93%. The proposed method was successfully applied for the extraction and preconcentration of trace acaricides in real fruit juice samples, and the results demonstrated the potential of the synthesized DESs for the extraction and determination of contaminants in aqueous samples.

CAS / MDL: 5137-55-3
研究领域: 分析化学 · 食品安全
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CHROMATOGRAPHIA · 2021 ·Vol. 84 ·期 11 ·1057-1064 · IF 2.044

Combination of Derivatization–HPLC–MS and Enzymatic Hydrolysis–Edman Degradation for Amino Acid Sequence and Configuration of Polymyxin B Components

Zhang Hanzhi,Li Feng,Dun Junling,Sun Ning,Liu Hao,Chen Guiliang

An analysis strategy that can simultaneously determine the amino acid site information and configuration for polymyxin (PM) components is reported in this study. The main components of PMB1, PMB2, and PMB1-I (the Leucine at position 7 changed to be Isoleucine) were purified from the mixture of PMB. The PMB component was hydrolyzed by hydrochloric acid to be a mixture of amino acids, which were derivatized with Marfey’s reagent of N α -(5-fluoro-2,4-dinitrophenyl)- l -alanine amide ( l -FDAA), and then, the configurations of amino acids were easily determined by HPLC–MS. However, the aforementioned method could not offer the information of amino acid at each site, a specific enzymatic hydrolysis method combined Edman degradation was developed. The fatty acyl-diaminobutyric acid (position 1) of PMB component was removed by ficin, and the PMB components were transformed to be PMB nonapeptide. The amino acids at each site of the nonapeptide were determined by N-terminal sequencing. Combining the results of the above methods, the amino acid information and configuration of each site in PM components can be determined, especially the l -Leucine and l -Isoleucine in PMB1 and PMB1-I. The workflow was useful for other PM analogues to identify the sequence and configuration for quality control.

CAS / MDL: 632-20-2 319-78-8
研究领域: 生物化学 · 药物分析 · 微生物学
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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

Highly sensitive analysis of fatty aldehydes in vegetable oils using a novel coumarin-based fluorescent probe by HPLC for quality control

Wenqing Zhang,Hao Zhu,Wenjie Xie,Chuanyuan Du,Xiuqiang Fang,Ruiming Zhang,Xiaosong Hu,Yawei Lin

A novel fluorescent probe , 3-(4-((hydroxylamino)methyl)-1H-pyrazol-1-yl)-7-methoxyl coumarin (HAPMC), has been designed and synthesized. The compound exhibits exceptional fluorescence properties due to a coumarin-pyrazolyl fluorophore. Moreover, it incorporates an N -hydroxylamine functional group capable of reacting with aldehydes to yield nitrone derivatives under mild conditions. This unique combination renders it an ideal derivatization reagent for aldehyde analysis. A standard method was established for the quantitative analysis of eight fatty aldehydes by utilizing high-performance liquid chromatography with fluorescence detection (HPLC-FLD) and a pre-column derivatization process, which has low detection limits (0.3–1.2 nM), satisfactory reproducibility (intraday and interday relative standard deviations in the range of 1.29 %-2.92 % and 1.73 %-3.45 %), and an extensive linear range (25–5000 nM) with excellent linearity (R 2  ≥ 0.9989). The spiked recoveries of the fatty aldehydes range from 89.6 % to 106.0 %. The greenness and sustainability of our approach are reinforced by evaluations conducted with the AGREE and RGB 12 algorithms. The established method was successfully applied to the qualitative and quantitative detection of fatty aldehydes in nine real vegetable oil samples, including peanut, canola, rice, soybean, olive, rapeseed, corn, sunflower, and blended oils. The fatty aldehydes are known to have adverse effects on human health due to their carcinogenic and mutagenic properties. The findings revealed that hexanal and nonanal were the most prevalent saturated fatty aldehydes, with a notable increase in the total aldehyde concentration observed as the temperature and duration of heating increased. Compared to alternative analytical techniques, this pre-column derivatization method utilizing HAPMC displayed simplicity, reliability, and sensitivity. The results demonstrate the potential for broad application of this approach in various important research domains, including food quality control, environmental monitoring, and medical research.

研究领域: 食品科学 · 分析化学 · 医学研究
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WATER ENVIRONMENT RESEARCH · 2022 ·Vol. 94 ·期 4 ·e10704 · IF 3.306

Activity measurement of arylsulfatase and β-glucuronidase in activated sludge: HPLC-based versus classical spectrophotometric method

Ke-meng Zhao,Shu-shu Zhong,Jun Zhang,Cun-sheng Zhang,Zhi Dang,Ze-hua Liu

Arylsulfatase and β-glucuronidase are two important enzymes in wastewater and surface water, which play important roles on cleavage of sulfate/glucuronide estrogens. In this work, a high-performance liquid chromatography (HPLC)-based new method was firstly established for arylsulfatase/β-glucuronidase with determination of p-nitrophenyl sulfate ( p NPS)/p-nitrophenyl-β-D-glucuronide ( p NPG). The limits of detections (LODs) of the developed method for pNPS and pNPG were 0.164 and 0.098 μM, respectively. Intraday and interday reproducibility expressed as relative standard deviation (RSD) values of retention times and peak areas was 0.39%–3.68% and 0.23%–4.74%, respectively. The respective recovery efficiencies of this HPLC-based method spiking at three different concentrations for p-nitrophenol ( p NP), p NPS, and p NPG in activated sludge were 76.5%–88.1%, 79.2%–93.1%, and 84.2%–96.1%, with RSD below 3.9%. The HPLC-based method was finally applied to estimate the enzyme activity of arylsulfatase/β-glucuronidase in one activated sludge system and along which the classical spectrophotometric method was also evaluated. Compared with the classic spectrophotometric analytical method, the HPLC-based new method could simultaneously measure arylsulfatase/β-glucuronidase one time, which was convenient and time-saving. Moreover, the developed method could effectively avoid possible underestimation that the spectrophotometric method might encounter. Practitioner points A new HPLC-based method for activity estimation of arylsulfatase and β-glucuronidase was developed. The HPLC-based method can simultaneously estimate enzyme activity of both arylsulfatase and β-glucuronidase. The HPLC-based method can avoid possible underestimation that spectrophotometric method may encounter.

CAS / MDL: 123-07-9 1643-19-2
研究领域: 环境生物学 · 生物化学 · 分析化学
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BIOMEDICAL CHROMATOGRAPHY · 2014 ·Vol. 29 ·期 6 ·860-868 · IF 1.662

HPLC/QTOF-MS/MS application to investigate phenolic constituents from Ficus pandurata H. aerial roots

Xiaoping Zhang,Huiqing Lv,Zuguang Li,Kezhi Jiang,Maw-Rong Lee

Ficus pandurata H. aerial roots are used as a traditional Chinese medicine for the treatment of uarthritis, indigestion and hyperuricemia. However, the bioactive constituents responsible for the pharmacological effects of F . pandurata H. are unclear. A simple and efficient HPLC/QTOF-MS/MS (high-performance liquid chromatography/electrospray ionization with quadrupole time-of-flight tandem mass spectrometry) method was established to detect and identify active constituents in the n -butanol extract of F . pandurata H. aerial roots. Chemical constituents were separated and investigated by HPLC/QTOF-MS/MS in the negative-ion mode. Thirty-seven compounds, including hydroxycinnamic acid derivatives, hydroxybenzoic acid derivatives, hydroquinone glycosides, flavonoid glycosides, etc., were identified or tentatively characterized in the n -butanol extract of F . pandurata H. aerial roots by comparing the UV spectra, accurate mass spectra and fragmentation pathways and retrieving the reference literatures. Moreover, the flavonoid trisaccharides and hydroxybenzoic acid derivatives were tentatively characterized in F . pandurata H. for the first time. The analytical tool used here is very valuable in the rapid separation and identification of the multiple and minor constituents in the n -butanol extract of F . pandurata H. aerial roots. Copyright © 2014 John Wiley & Sons, Ltd.

研究领域: 药理学 · 分析化学 · 植物化学
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