JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2025
·
IF 4.6
Lingling Zhao,Xinqi Pan,Jie Shi,Hua Ye,Huanan Guan,Yuanxin Guo,Jian-Jun Zhong
Urocanic acid, like histamine, is a degradation product of histidine that may accumulate over the storage of histidine-rich pelagic fish. Recently evidence from the dermatological and related fields has directed the attention of food scientists toward the adverse health effects of urocanic acid, mostly as a possible “missing factor” responsible for scombrotoxicosis besides histamine. However, experimental effort to study the hypothesis remains scarce, especially regarding the formation of urocanic acid in comparison to the well-documented histamine. Here we report a mixed-mode HPLC method for simultaneously analyzing urocanic acid (both the trans - and cis -isomers), histamine, and histidine in chub mackerel ( Scomber japonicus ) fillets and the use of the method to monitor their changes in concentration at typical refrigeration and abuse temperatures. The method features a simple, reliable chromatographic analysis in cation-exchange/reversed-phase/hydrophilic-interaction triple mode of retention, without the need of precolumn derivatization or addition of ion-pairing agents. At both 4 and 20 °C slow but consistent formation of trans -urocanic acid was observed over time with a relatively faster rate at 20 °C. Histamine formation, by contrast, occurred at 20 °C but ceased completely at 4 °C. In addition, we demonstrate the occurrence of trans -to- cis isomerization of UCA in chub mackerel fillets upon direct sunlight exposure: under our conditions, an isomerization yield around 13 % was achieved within hours on a sunny winter day. Overall, this study provides a chemical analysis method and relevant data for exploring the possible role of urocanic acid in the aetiology of scombrotoxicosis.
研究领域:
食品科学
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生物化学
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2015
·
IF 2.729
Huiqing Zou,Mingfeng Xiang,Xinming Ye,Yuanzhen xiong,Baogang Xie,Jianghua Shao
Serum uric acid (UA) concentration is positively associated with proteinuria. However, the relationship between proteinuria and urinary metabolites of purine metabolism remains unknown. This study developed a hydrophilic interaction chromatography (HILIC)-based HPLC method with ultraviolet detection (UV) to quantify creatinine (Cr), UA, xanthine, and hypoxanthine in human urine simultaneously. The urinary concentrations of UA and Cr obtained by our method are consistent with those measured by an autoanalyzer. The HPLC-HILIC-UV method was validated as selective and robust with simple sample preparation for measuring UA, xanthine, hypoxanthine and Cr, which is suitable for large clinical studies. The UA/Cr ratios in random urine samples were 5.5 times lower in proteinuria patients (0.077 ± 0.008) than in healthy individuals (0.424 ± 0.037). Moreover, the UA/hypoxanthine ratio in proteinuria patients was approximately 10 times lower than that in healthy individuals. Our findings revealed a reduced urinary UA excretion, which is one of the factors leading to increased serum UA in proteinuria patients.
研究领域:
医学
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生物化学
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DOI
高影响因子
Chinese Journal of Natural Medicines
·
2021
·
IF 3
Zheng-Ming QIAN,Zi WU,Qi HUANG,Chuan-Xi WANG,Guo-Yin TAN,Wen-Jia LI,Wan-Yang SUN,Gen-Pin LV,Hao GAO
An eco-friendly and fast HPLC method was developed for the determination of adenosine, inosine, guanosine and uridine in Cordyceps and related products (fermented mycelia of Hirsutella sinensis and Paecilomyces hepiali ). The sample was ultrasonically extracted using 0.5% phosphoric acid solutions for 2.5 min. Sample separation was performed on a Poroshell SB-Aq column (50 mm × 4.6 mm, 2.7 μm) using eco-friendly mobile phase consisting of formic acid and ammonium formate aqueous solution at a flow rate of 1.0 mL·min −1 . The detection wavelength was 260 nm. The developed HPLC method showed good linearity with correlation coefficients of 1.0000 in the test range. Good precision, repeatability and stability of this method were also observed (RSD ≤ 2.81%). The recovery ranged from 91.84%−105.19% (RSD ≤ 2.59%). Compared with reported methods, the current method did not use harmful organic solvent and took only 10.5 min. It obtained a high eco-score of 91 by the “Analytical Eco-Scale” tool. The developed method is eco-friendly and fast, which is suitable for the quality evaluation of Cordyceps and related products.
研究领域:
药学
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分析化学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2015
·Vol. 30
·期 4
·601-605
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IF 1.723
Zhaoli Ling,Ping Xu,Zeyu Zhong,Fan Wang,Nan Shu,Ji Zhang,Xiange Tang,Li Liu,Xiaodong Liu
A new pre-column derivative high-performance liquid chromatography (HPLC) method for determination of d -glucose with 3- O -methyl- d -glucose (3-OMG) as the internal standard was developed and validated in order to study the gluconeogenesis in HepG2 cells. Samples were derivatized with 1-phenyl-3-methy-5-pyrazolone at 70°C for 50 min. Glucose and 3-OMG were extracted by liquid–liquid extraction and separated on a YMC-Triart C 18 column, with a gradient mobile phase composed of acetonitrile and 20 m m ammonium acetate solution containing 0.09% tri-ethylamine at a flow rate of 1.0 mL/min. The eluate were detected using a UV detector at 250 nm. The assay was linear over the range 0.39–25 μ m ( R 2 = 0.9997, n = 5) and the lower limit of quantitation was 0.39 μ m (0.070 mg/mL). Intra- and inter-day precision and accuracy were <15% and within ±3%, respectively. After validation, the HPLC method was applied to investigate the gluconeogenesis in Dulbecco's modified Eagle medium (DMEM) cultured HepG2 cells. Glucose concentration was determined to be about 1–2.5 μ m in this gluconeogenesis assay. In conclusion, this method has been shown to determine small amounts of glucose in DMEM successfully, with lower limit of quantitation and better sensitivity when compared with common commercial glucose assay kits. Copyright © 2015 John Wiley & Sons, Ltd.
研究领域:
生物化学
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医学检测
·
药理学
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DOI
PubMed
高影响因子
Drug Research
·
2019
·Vol. 70
·期 01
·12-22
·
IF 0
Chaowei Zhang,Chengqun Han,Lili Sun,Jinlong Yu,Qiaogen Zou
Bepotastine besilate (here after referred to as BTST), chemically known as ({d(S)4[4[(4chlorophenyl) (2pyridyl) methoxy] piperidino} butyric acid monobenzene sulphonate), is a second-generation antihistamine drug. To the best of our knowledge, no studies concerning the isolation or identification of process-related impurities have been reported so far. The current study reports the development and validation of a stability-indicating RP-HPLC method for the separation and identification of 5 potential impurities in bepotastine besilate. In this experiment, the structures of 3 process-related impurities were found to be new compounds. They were characterized and confirmed by NMR and MS spectroscopy analyses. These 3 new compounds were proposed to be (S)-4-[(phenyl)-2-pyridinylmethoxy]-1-piperidinebutanoic acid,(Imp-A); 4-[(S)-(4-chlorophenyl)-2-pyridinylmethoxy]-1- piperidinebutyric acid, N-oxide (Imp-B) and (S)-4-[(4- chlorophenyl)-2-pyridinylmethoxy]-1-piperidylethane (Imp-C). In addition, an efficient optimized chromatographic method was performed on a Shimadzu Inertsil C8–3 column (150 mm×4.6 mm, 3 μm) to separate and quantify these 5 impurities. It was using 15 mmol ammonium formate buffer in water (pH adjusted to 3.8 with formic acid) and acetonitrile as the mobile phase in gradient mode. The method was developed to separate and quantify these 5 impurities obtained in the range of 0.05–0.75 μg/mL. It was validated and proven to be selective, accurate and precise and suitable. It is the first publication of identification and characterization data of the 3 new compounds. It is also the first effective HPLC method for separation and quantification of all of process-related impurities in bepotastine besilate.
研究领域:
药物化学
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分析化学
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产品关联
DOI
PubMed
JOURNAL OF AOAC INTERNATIONAL
·
2019
·Vol. 100
·期 4
·1029-1037
·
IF 1.201
Zou Liang,Sun Lili,Zhang Hui,Hui Wenkai,Zou Qiaogen,Zhu Zheying
The characterization of process-related impurities and degradation products of safinamide mesilate (SAFM) in bulk drug and a stability-indicating HPLC method for the separation and quantification of all the impurities were investigated. Four process-related impurities (Imp-B, Imp-C, Imp-D, and Imp-E) were found in the SAFM bulk drug. Five degradation products (Imp-A, Imp-C, Imp-D, Imp-E, and Imp-F) were observed in SAFM under oxidative conditions. Imp-C, Imp-D, and Imp-E were also degradation products and process-related impurities. Remarkably, one new compound, identified as (S)-2-[4-(3-fluoro-benzyloxy) benzamido] propanamide (i.e., Imp-D), is being reported here as an impurity for the first time. Furthermore, the structures of the aforementioned impurities were characterized and confirmed via IR, NMR, and MS techniques, and the most probable formation mechanisms of all impurities proposed according to the synthesis route. Optimum separation was achieved on an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm), using 0.1% formic acid in water (pH adjusted to 5.0) and acetonitrile as the mobile phase in gradient mode. The proposed method was found to be stability-indicating, precise, linear, accurate, sensitive, and robust for the quantitation of SAFM and its process-related substances, including its degradation products.
研究领域:
药物化学
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分析化学
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产品关联
DOI
PubMed
高影响因子
Journal of Analytical Methods in Chemistry
·
2020
·
IF 1.878
Bo Tao,Gang Wang,Zongning Yin,Xiaocong Pu,Yan Jiang,Luohong Zhang,Jie Cheng,Yong Li,Jiayu Zhang
The infusion bag is mainly made up of polyolefin polymer. Antioxidants are usually added to these polymer materials in the production process to prevent the materials from aging and enhance the stability of the materials. Because of the potential harm of antioxidants to human body, it is necessary to limit the amount of antioxidants migrating to the pharmaceutical solutions. In the present study, we developed and validated the HPLC method for the simultaneous quantification of antioxidants and their degradation products migrating to sodium chloride solution for injection. A total of six antioxidants and six their degradation products were separated and simultaneously determined by using a Waters Symmetry RP18 column (250 × 4.6 mm, 5 μm) and gradient elution of methanol/acetonitrile/acetic acid-water (1 : 99, v/v) at a flow rate of 1.0 mL/min. The detective wavelength was set at 277 nm, and the column temperature was maintained at 35°C. The method was validated in terms of limit of detection (LOD, 0.011–0.151 μg/mL), limit of quantification (LOQ, 0.031–0.393 μg/mL), intraday precision (0.25%–3.17%), interday precision (0.47%–3.48%), linearity (0.1–46.8 μg/mL, r > 0.9994), stability (0.35%–3.29%), and accuracy (80.39%–104.31%). In the extraction experiment, antioxidants, BHT, 1010, 1330, 1076, and 168, and their degradation products, 1310 and DBP, were detected in the packaging materials. Only 1310 was detected in the migration experiment. The maximum daily dosage of sodium chloride for blood transfusion is three bags, and the content of 1310 in long-term testing samples is from 0 to 12 months ranging from 37.44 μg/3 bags to 48.71 μg/3 bags. The daily intake of 1310 did not exceed 48.71 μg, which was much lower than its permitted daily exposure (PDE, 300 μg/day). Therefore, the antioxidants and their degradation products migrating into the drug solution would not cause drug safety risks.
研究领域:
药学
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分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2015
·Vol. 54
·期 3
·353-360
·
IF 1.363
Zhou Yuxia,Zhou Fan,Yan Fei,Yang Feng,Yao Yuxian,Zou Qiaogen
Eleven potential impurities, including process-related compounds and degradation products, have been analyzed by comprehensive studies on the manufacturing process of clevidipine butyrate. Possible formation mechanisms could also be devised. MS and NMR techniques have been used for the structural characterization of three previously unreported impurities (Imp-3, Imp-5 and Imp-11). To separate and quantify the potential impurities in a simultaneous fashion, an efficient and advanced RP-HPLC method has been developed. In doing so, four major degradation products (Imp-2, Imp-4, Imp-8 and Imp-10) can be observed under varying stress conditions. This analytical method has been validated according to ICH guidelines with respect to specificity, accuracy, linearity, robustness and stability. The method described has been demonstrated to be applicable in routine quality control processes and stability evaluation studies of clevidipine butyrate.
研究领域:
药物化学
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分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Chunwang Fu,Fan Jiang,Kun Gao,Xiaobai Xue,Shuo Lei,Chunting Liu,Huan Yu,Hui Wang,Xiaoqian Dong,Jian Jiao,Guojie Liu,Qiang Yang
Although the secondary packing materials do not directly contact the finished drug products, compound migration may still happen between them. To ensure drug quality and safety, extractables and leachables of the packing materials should be analyzed. In this study, 2,6-di-tert-butyl-4-methylphenol (BHT) was first found in the labels for pharmaceutical packaging. For the identification of the compound, a strategy combining high performance liquid chromatography (HPLC), ultra-performance liquid chromatography-quadrupole time-of-flight mass (UPLC-Q-TOF-MS) and nuclear magnetic resonance (NMR) spectroscopy was utilized. Afterwards, a effective and sensitive HPLC method for quantification of BHT was developed and validated. Finally, a toxicological risk assessment of BHT was performed to ensure the safety of drugs.
研究领域:
药学
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分析化学
·
毒理学
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产品关联
DOI
PubMed
高影响因子
WATER ENVIRONMENT RESEARCH
·
2022
·Vol. 94
·期 4
·e10704
·
IF 3.306
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.
研究领域:
环境生物学
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生物化学
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分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2016
·
IF 3.169
Yidi Yang,Xi Zhu,Fei Zhang,Wei Li,Ying Wu,Li Ding
Stress testing was carried out under acidic, alkaline, oxidative, thermal and photolytic conditions to evaluate the intrinsic stability of posaconazole injection. A total of four degradation products were detected and the drug was found to be susceptible to oxidative and thermal degradations. Three unknown degradants formed under oxidative stress condition were isolated by preparative HPLC and unambiguously elucidated by LC–TOF/MS, LC–MS/MS, 1 H NMR, 13 C NMR and 2D NMR techniques. Based on the spectrometric and spectroscopic information, these novel degradation products were unequivocally assigned as the N-oxides of posaconazole. Probable mechanisms for the formation of the degradants were proposed. A new and selective HPLC method was developed and validated to separate, detect and quantify all the degradants in posaconazole injection.
研究领域:
药物分析
·
药学
·
质谱分析
·
核磁共振
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Xinran Zhang,Mohamed Abdulbagi,Limin Wang,Jiafeng Wang,Bin Di,Bo Li
Amino acid epimerization , a process of converting L -amino acids to D -amino acids, will lead to modification in the protein structure and, subsequently, its biological function . This modification causes no change in protein m/z and may be overlooked during protein analysis . Aspartic Acid Epimerization (AAE) is faster than other amino acids and could be accelerated by free radicals and peroxides. In this work, a novel and site-specific HPLC method using a chiral stationary phase for determining the AAE in the active site model peptide (AP) of Peroxiredoxin 2 has been developed and validated. The developed method showed good linearity (1 – 200 μg/mL) and recoveries of the limit of quantification (LOQ), low, medium, and high concentrations were between 85% and 115%. The Kinetics of AAE in AP were studied using the developed method, and the results showed that when ascorbic acid and Cu 2+ coexisted, the AP epimerized rapidly. The AAE extent increased with time and was positively correlated with hydrogen peroxide generation.
研究领域:
生物化学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）