JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2024
·
IF 4
Jian-Jun Zhong,Lingling Zhao,Yuanxin Guo,Zhanming Li,Hua Ye,Huanan Guan,Zhiqiang Xing,Weiqing Wang
The coffee phytochemical trigonelline and its roasting products nicotinic acid and N -methylpyridinium represent an important class of bioactives that mediate the health benefits of coffee consumption. However, there is a paucity of methods for their simultaneous analysis in coffee beans, especially those affordable and reliable for widespread routine use. To improve this situation, an easy-to-use HPLC−UV method was developed in this study based on a reversed-phase/cation-exchange mixed-mode column showing unique chromatographic selectivity toward the polar and ionic analytes over the matrix components of coffee. The selectivity was achieved by using a decreasing acetonitrile gradient, which tuned the column to a cation-exchange/hydrophilic interaction (CEX/HILIC) mixed separation mode whilst minimizing its hydrophobic interaction capability. The method was assessed for figures of merit, giving limits of detection in coffee beans at around the 0.1 mg/100 g wet matter level, and verified for its applicability to a heterogeneous set of coffee bean samples differing in roasting degree and origin.
研究领域:
分析化学
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食品科学
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植物化学
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高影响因子
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2018
·
IF 0.827
Zhiwei Sun,Qianqian Jin,Yanxin Yu,Jie Cheng,Zhongyin Ji,Guoliang Li,Jinmao You
Urinary aromatic diamines are exposure biomarkers of diisocyanate which are highly irritating to skin, mucosa and the upper respiratory system. In this study, a highly sensitive and selective high-performance liquid chromatography-fluorescence detection (HPLC-FLD) method was developed for determination of three aromatic diamines, 4,4′-methylenedianiline (MDA), 2,4-toluenediamine (4TDA) and 2,6-toluenediamine (6TDA) exposed to corresponding diisocyantes in human urine. The whole idea is based on an intramolecular excimer-forming fluorescence derivatization using 4-(1-pyrene)butanoyl chloride (PBC), followed by performing HPLC-FLD analysis.The resulting polypyrene-labeled derivatives of these aromatic diamines provided intramolecular excimer fluorescence at the emission wavelength of 475 nm wavelengths, which was shifted markedly to the higher emission wavelengths as compared with the wavelengths of the pyrene monomer. Under this condition, interferences such as amino acids and biogenic monoamines gave no peaks. It was found that using PBC derivatization, it was possible to improve the sensitivity and selectivity toward aromatic diamines. The limits of detection (LODs) were in the range of 0.30–0.52 ng/L, while the limits of quantitation (LOQs) between 1.05 and 1.63 ng/L. The intraday and interday precision was in the range of 3.6–4.5% and 4.1–5.7%, respectively. The proposed method was successfully applied to the quantitation of these exposure biomarkers in human urine samples.
研究领域:
分析化学
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职业健康
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环境毒理学
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DOI
高影响因子
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
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2018
·Vol. 19
·期 2
·443
·
IF 3.687
Mengsha Li,Rui Guo,Fei Yu,Xu Chen,Haiyan Zhao,Huixin Li,Jun Wu
Arthrobacter pascensZZ21 is a plant-beneficial, fluoranthene-degrading bacterial strain found in the rhizosphere. The production of the phytohormone indole-3-aectic acid (IAA) by ZZ21 is thought to contribute to its ability to promote plant growth and remediate fluoranthene-contaminated soil. Using genome-wide analysis combined with metabolomic and high-performance liquid chromatography-mass spectrometry (HPLC-MS) analyses, we characterized the potential IAA biosynthesis pathways inA. pascensZZ21. IAA production increased 4.5-fold in the presence of 200 mg·L−1tryptophan in the culture medium. The transcript levels ofprrandaldH, genes which were predicted to encode aldehyde dehydrogenases, were significantly upregulated in response to exogenous tryptophan. Additionally, metabolomic analysis identified the intermediates indole-3-acetamide (IAM), indole-3-pyruvic acid (IPyA), and the enzymatic reduction product of the latter, indole-3-lactic acid (ILA), among the metabolites of ZZ21, and subsequently also IAM, ILA, and indole-3-ethanol (TOL), which is the enzymatic reduction product of indole-3-acetaldehyde, by HPLC-MS. These results suggest that the tryptophan-dependent IAM and IPyA pathways function in ZZ21.Keywords:Arthrobacter;IAA biosynthesis pathway;genome-wide analysis;metabolomics;HPLC-MS
研究领域:
植物学
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微生物学
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环境科学
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DOI
PubMed
高影响因子
MOLECULES
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2024
·Vol. 29
·期 3
·567
·
IF 4.2
Yayun Guo,Zhe Wang,Yi He,Huanhuan Gao,Hongmei Shi
Aspergillus carbonariusis known to produce the carcinogenic ochratoxin A (OTA) in grapes. The metabolism process before OTA biosynthesis influences the content and composition of the volatile compounds in grapes. In this study, a self-established method based on QuEChERS coupled with high-performance liquid chromatography–fluorescence detection (HPLC-FLD) was used to determine the OTA levels during a seven-day contamination period. The results showed that OTA was detected on the second day after contamination withA. carbonarius. Thus, the first day was considered as the critical sampling timepoint for analyzing the volatiles in grapes before OTA biosynthesis. Additionally, the volatile compounds in grapes were analyzed using headspace solid-phase microextraction gas chromatography–mass spectrometry (HS-SPME-GC-MS) and dispersive liquid–liquid microextraction gas chromatography–mass spectrometry (DLLME-GC-MS). The corresponding data were evaluated via multivariate data analysis using projection methods, including PCA and OPLS-DA. The results indicated significant differences in the nine volatile compounds in grapes contaminated withA. carbonariusbefore OTA biosynthesis. The results of the Pearson correlation analysis showed positive correlations between ethyl acetate, styrene, 1-hexanol and OTA; (E)-2-hexenal and nerolic acid were negatively correlated with OTA. Overall, these findings provide a theoretical basis for the early prediction of OTA formation in grape and grape products using GC-MS technology.Keywords:volatile compounds;Ochratoxin A;QuEChERS-HPLC-FLD;HS-SPME-GC-MS;DLLME-GC-MS;OPLS-DA
研究领域:
食品科学
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真菌学
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分析化学
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DOI
PubMed
高影响因子
CHROMATOGRAPHIA
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2025
·Vol. 88
·期 11
·891-903
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IF 1.3
Li Wei-Si,Zhang Zhe-Meng,Wang Xue-Ying,Sun Chun-Xia,Liu Zhen,Ma Xiao,Qiao Zhou,Zhu Hai-Bin,Han Ling-Fei
Esomeprazole magnesium (EMO) is the S -enantiomer of omeprazole. As a second-generation proton pump inhibitor, it is more effective than omeprazole in inhibiting gastric acid secretion. Therefore, it is of great necessity to establish a quality control method to support its pharmaceutical development. The starting materials for the preparation of EMO may contain six potential genotoxic impurities (PGIs), designated as RC16, RC17, RC18, RC20, RC21, and RC23. These impurities have similar chemical structures, all containing benzene rings or pyridine rings with small differences in substituents, which leads to similar retention behaviors in the chromatographic column, and peak overlap is likely to occur during HPLC analysis, making it impossible to accurately determine the content of impurities. To enhance the quality control, this study established a sensitive and specific HPLC–MS/MS method. Utilizing electrospray ionization (ESI) in positive multiple reaction monitoring (MRM) mode, this method was used to determine the trace amounts of six PGIs in EMO raw material. On a 40 °C Inertsil ODS-SP C18 chromatographic column (4.6 × 150 mm, 5 μm), the six PGIs were well separated in an equilibrated elution mode at a flow rate of 0.5 mL min⁻ 1 . 0.5% formic acid in water and methanol were used as the mobile phase A and B, respectively. The method was rigorously validated in terms of precision, accuracy, limit of detection, limit of quantification, linear range, and robustness, and with all parameters meeting pre-defined acceptance criteria. Graphical
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高影响因子
MOLECULES
·
2022
·Vol. 27
·期 9
·2684
·
IF 4.927
Ziqi Qian,Yi Wang,Shuyu Shen,Wenyang Tao,Yu Zhang,Xingqian Ye,Shiguo Chen,Haibo Pan
Proanthocyanidins (PACs) have been proven to possess a wide range of biological activities, but complex structures limit their study of structure–function relationships. Therefore, an efficient and general method using hydrophilic interaction high-performance liquid chromatography coupled with high-resolution quadrupole time-of-flight tandem mass spectrometry (HILIC-QTOF-MS) was established to analyze PACs from different plant materials. This method was successfully applied to characterize PACs from Chinese bayberry (Myrica rubraSieb. et Zucc.) leaves (BLPs), sorghum testa (STPs) and grape seeds (GSPs). BLPs with the degree of polymerization (DP) from 1 to 8 were separated. BLPs are mainly B-type prodelphinidins and A-type BLPs were first found in this study. STPs and GSPs belonging to procyanidins showed DP from 3 to 11 and 2 to 12, respectively. A-type linkages were found for every DP of STPs and GSPs, which were first found. These results showed that HILIC-QTOF-MS can be successfully applied for analyzing PACs from different plant materials, which is necessary for the prediction of their potential health benefits.Keywords:Chinese bayberry leaves;sorghum testa;grape seeds;proanthocyanidins;HILIC-QTOF-MS
研究领域:
植物化学
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分析化学
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DOI
PubMed
高影响因子
Applied Sciences-Basel
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2025
·Vol. 15
·期 3
·1486
·
IF 2.5
Mengye Jia,Riya Jin,Yina Qiao,Yu Jiang,Jiaoqin Liu,Zengdi He,Zhaoguo Liu,Jingshuai Gao
2,2′,4,4′,6,6′-hexanitrostilbene (HNS) is a heat-resistant, low-sensitivity energetic material with widespread applications in pliable linear-shaped charges, high-temperature-resistant oil well perforating charges, and rocket propellants. However, the presence of highly toxic and mutagenic nitroaromatic compounds in HNS wastewater necessitates efficient and accurate detection methods. Unfortunately, the existing analytical methods for HNS detection are outdated and incompatible with modern equipment. This limits their application due to issues with detection range, accuracy, and cost. To address this gap, an improved method was developed using an Ultimate 3000 UHPLC system with methanol and water as the mobile phase and UV-Vis detection at 271 and 226 nm wavelengths. The results indicate that the optimal detection conditions are achieved with a methanol-to-water ratio of 70:30 and a flow rate of 0.5 mL/min, providing high accuracy and efficiency. Compared to traditional methods, this approach reduced the detection time by nearly 70%, with the shortest analysis time ranging from 6 to 6.5 min, significantly lowering the cost of HNS detection. The method demonstrated excellent linearity (R2> 0.9999) and high sensitivity within the concentration range of 0.50–150.00 mg/L, with precise and reliable results. This work provides both theoretical insights and experimental validation for the detection and analysis of HNS in wastewater.
研究领域:
分析化学
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环境科学
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含能材料
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色谱学
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DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
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2017
·Vol. 41
·期 4
·877-885
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IF 2.557
Dan Liu,Ting Qiao,Haiyan Liu,Xiaoling Wang,Zhi-guo Shi
In the present study, a polar-embedded reversed-phase liquid chromatographic stationary phase that contained internal sulfone groups was prepared. The synthesis involved the “thiol-ene” click chemistry between the vinyl functionalized silica and 1-octadecanethiol, followed by the oxidization of sulfide to sulfone groups. The resulting material simultaneously possessed the alkyl chain, i.e. C18, and the internal sulfone groups. Elemental analysis demonstrates that the element contents of the C18/sulfone silica were C 8.94%, H 1.87% and S 0.66%. Chromatographic evaluations indicate that the C18/sulfone stationary phase exhibited a little less retention than the C18/sulfide one. A comparable chromatographic performance of neutral analytes was obtained on these two columns, but much better chromatographic performance in the case of basic and acid analytes was obtained on C18/sulfone stationary phase with additional features such as lower silanol activity, better stability (stable working conditions of pH 1.0–10.0), and better compatibility with 100% aqueous mobile phases. The batch-to-batch reproducibility was acceptable (the RSDs of retention times for the probes were no higher than 1.73%), demonstrating the suitability of the applied synthetic strategy for the new stationary phase. The C18/sulfone is a promising polar-embedded RPLC stationary phase.
研究领域:
分析化学
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材料科学
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DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2014
·Vol. 407
·期 6
·1595-1605
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IF 3.578
Du Yan,Wu Dapeng,Wu Qian,Guan Yafeng
In this study, the efficiency of five peptide-extraction methods—acetonitrile (ACN) precipitation, ultrafiltration, C18 solid-phase extraction (SPE), dispersed SPE with mesoporous carbon CMK-3, and mesoporous silica MCM-41—was quantitatively investigated. With 28 tryptic peptides as target analytes, these methods were evaluated on the basis of recovery and reproducibility by using high-performance liquid chromatography–triple-quad tandem mass spectrometry in selected-reaction-monitoring mode. Because of the distinct extraction mechanisms of the methods, their preferences for extracting peptides of different properties were revealed to be quite different, usually depending on the pI values or hydrophobicity of peptides. When target peptides were spiked in bovine serum albumin (BSA) solution, the extraction efficiency of all the methods except ACN precipitation changed significantly. The binding of BSA with target peptides and nonspecific adsorption on adsorbents were believed to be the ways through which BSA affected the extraction behavior. When spiked in plasma, the performance of all five methods deteriorated substantially, with the number of peptides having recoveries exceeding 70 % being 15 for ACN precipitation, and none for the other methods. Finally, the methods were evaluated in terms of the number of identified peptides for extraction of endogenous plasma peptides. Only ultrafiltration and CMK-3 dispersed SPE performed differently from the quantitative results with target peptides, and the wider distribution of the properties of endogenous peptides was believed to be the main reason.
Distribution of the recoveries of target peptides after treatment by the five peptide-extraction methods
研究领域:
生物化学
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分析化学
·
蛋白质组学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2019
·Vol. 42
·期 24
·3646-3652
·
IF 2.516
Yao Sun,Pengfei Li,Ting Wang,Liting Qin,Gege Cheng,Liqun Shen,Xingdong Yao,Shaoping Wei,Jianxin Jiang,Fuhou Lei
Alkaloids are important natural products that exhibit a wide spectrum of pharmacological activities. To efficiently separate and purify them, a rosin-based polymer-bonded silica stationary phase in high-performance liquid chromatography was synthesized via the surface radical polymerization of ethylene glycol maleic rosinate acrylate and methacrylic acid onto functionalized silica. The stationary phases, columns, optimization of chromatographic conditions for alkaloids, and thermodynamic behavior of the analytes on the column were fully studied. Under the optimized conditions, the prepared column efficiently purified natural camptothecine, caffeine, and evodiamine with the corresponding purities of 92, 96, and 97%. With this work, we have developed an efficient approach to isolate alkaloids and promoted the research on rosin-based materials in biomedicine and analytical chemistry.
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DOI
PubMed
高影响因子
Natural Products and Bioprospecting
·
2019
·Vol. 9
·期 3
·201-208
·
IF 0
Liu Qi,Chi Quan,Fan Ru-Ting,Tian Hui-Dong,Wang Xian
Abstract A sensitive and rapid high performance liquid chromatography–mass spectrometry (HPLC–MS) method was developed and validated for simultaneous quantification of ten steroid hormones, including estrogens, androgens, progesterones, and corticosteroids four classes of steroids. The following ten steroid hormones were analyzed: progesterone, 21-deoxycortisol, estrone, 4-androstenedione, testosterone, dihydro-testosterone, androstenone, dehydroepiandrosterone, corticosterone and cortisone. Stable deuterated isotopes were used as internal standards for quantification. Sample preparation with and without derivatization were performed after liquid–liquid extraction, and the corresponding results were compared according to sensitivity and selectivity. Hydroxylamine derivatization was found to improve the ionization efficiency of the analytes for electrospray ionization MS analysis. The gradient of mobile phase and experimental parameters for HPLC separation were optimized. The lower limits of quantification were in the range of 0.05–5 ng mL −1 with wide linear range for the ten steroid hormones. The intra-day precision < 11.1% and recovery of 84.5–120% with negligible matrix effect were achieved, where within the acceptance limits of the FDA guideline. Total HPLC–MS analysis time was 6 min. This method enables simultaneous quantification of steroids in human serum. It will be helpful for the serum steroid profiling in order to understand various endocrinology diseases. Graphical Abstract
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PubMed
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Wenchan Deng,Rongrong Huang,Yuanjiang Pan,Cuirong Sun
The metabolism process of amino acids is closely related to the growth of normal and cancer cells. It is still not clear how L/D-configuration amino acids participate in the metabolism of colorectal cell. Herein, intra- and extra-cellular metabolic distribution of L/D-amino acids in colorectal cell (HCT116) and human normal intestinal epithelial cell (NCM460) were profiled utilizing HPLC-MS/MS coupled with a chiral probe. The results displayed the differential metabolic portrayal for the two cell lines. Compared with NCM460 cell, 13 kinds of significant differential amino acids were founded in a lower concentration within HCT116 cell, and L-Gln was even not detected for intra-cell; as for extra-cell culture medium, the HCT116 cell consumed more L-Gln, D-Phe and D-Leu, while L-Met was low ingested in HCT116 cell. L-Ala and Gly were excretion in both two cell lines, excepted L-Cit which was uptake in HCT116 and excretion in NCM460 cell. Furthermore, the dynamic changes of chiral amino acids displayed that phenylalanine, tyrosine and tryptophan biosynthesis and arginine biosynthesis is the major pathway for intra-cellular metabolites and extra-cellular metabolites, respectively. Moreover, with additional D-amino acids in culture medium, the results exhibited that high concentration of D-amino acids have no significant effect on the proliferation of NCM460 cell, but could influence the profiling of amino acids metabolites, and further affect the proliferation of HCT116 cell. This present work enhances the understanding of these differential amino acids metabolic network and depicts a dynamic process of metabolic dysregulation of HCT116 and NCM460 cell.
研究领域:
生物化学
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肿瘤学
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产品关联
DOI
PubMed
高影响因子
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