JOURNAL OF SEPARATION SCIENCE
·
2019
·Vol. 42
·期 20
·3234-3242
·
IF 2.516
Zi-Ling Li,Na Li,Li Du,Ya-Hui Wang,Bo Fang,Man-Man Wang,Qian Wang
The biomonitoring of hydroxy polycyclic aromatic hydrocarbons in urine, as a direct way to access multiple exposures to polycyclic aromatic hydrocarbons, has raised great concerns due to their increasing hazardous health effects on humans. Solid-phase extraction is an effective and useful technique to preconcentrate trace analytes from biological samples. Here, we report a novel solid-phase extraction method using a graphene oxide incorporated monolithic syringe for the determination of six hydroxy polycyclic aromatic hydrocarbons in urine coupled with liquid chromatography-tandem mass spectrometry. The effect of graphene oxide amount, washing solvent, eluting solvent, and its volume on the extraction performance were investigated. The fabricated monoliths gave higher adsorption efficiency and capacity than the neat polymer monolith and commercial C 18 sorbent. Under the optimum conditions, the developed method provided the detection limits ( S/N = 3) of 0.02–0.1 ng/mL and the linear ranges of 0.1–1500 ng/mL for six analytes in urine sample. The recoveries at three spiked levels ranged from 77.5 to 97.1%. Besides, the intra column-to-column ( n = 3) and inter batch-to-batch ( n = 3) precisions were ≤ 9.8%. The developed method was successfully applied for the determination of hydroxy polycyclic aromatic hydrocarbons in urine samples of coke oven workers.
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CHIRALITY
·
2018
·Vol. 30
·期 12
·1277-1286
·
IF 1.833
Lu-Ning Sun,Yi-Wen Shen,Yu-Wen Ying,Duo Li,Teng-Fei Li,Xue-Hui Zhang,Ping Zhao,Li Ding,Yong-Qing Wang
Rabeprazole is an effective proton pump inhibitor to treat acid-related diseases. To achieve the simultaneous determination of rabeprazole enantiomers in human plasma, a chiral LC-MS/MS method was developed and validated. Acetonitrile including 0.1% ammonium were used as protein precipitating agent. Analytes were separated within 8 minutes on a Chiralpak IC column (4.6 mm × 150 mm, 5 μm). The mobile phase was 10 mM ammonium acetate including 0.2% acetic acid-acetonitrile (35:65, v/v). An API 4000 mass spectrometer was used as detector for the analysis, and the multiple reactions monitoring transitions of m/z 360.1 → 242.2 and 346.1 → 198.1 were opted for quantifying rabeprazole enantiomers and internal standard. Matrix effects were not apparent for each enantiomer and internal standard (esomeprazole), the calibration curves were linear over the concentration of 0.500 to 400 ng·mL −1 , the intra-run precisions were below 5.4%, the inter-run precisions were below 9.9%, and the accuracy was between −9.2% and 9.3%. There was no chiral inversion observed during sample storage, preparation procedure, and analysis, demonstrating that analytes were stable in this study. This method was applied to the stereoselective pharmacokinetic study of (R)-(+)- and (S)-(−)-rabeprazole after oral administration of 10-mg rabeprazole sodium enteric-coated tablet in healthy Chinese subjects.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2015
·Vol. 407
·期 24
·7359-7368
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IF 3.436
Zhao Zhiyong,Liu Na,Yang Lingchen,Deng Yifeng,Wang Jianhua,Song Suquan,Lin Shanhai,Wu Aibo,Zhou Zhenlei,Hou Jiafa
Mycotoxins have the potential to enter the human food chain through carry-over of contaminants from feed into animal-derived products. The objective of the study was to develop a reliable and sensitive method for the analysis of 30 mycotoxins in animal feed and animal-derived food (meat, edible animal tissues, and milk) using liquid chromatography–tandem mass spectrometry (LC–MS/MS). In the study, three extraction procedures, as well as various cleanup procedures, were evaluated to select the most suitable sample preparation procedure for different sample matrices. In addition, timed and highly selective reaction monitoring on LC–MS/MS was used to filter out isobaric matrix interferences. The performance characteristics (linearity, sensitivity, recovery, precision, and specificity) of the method were determined according to Commission Decision 2002/657/EC and 401/2006/EC. The established method was successfully applied to screening of mycotoxins in animal feed and animal-derived food. The results indicated that mycotoxin contamination in feed directly influenced the presence of mycotoxin in animal-derived food.
Multi-mycotoxin analysis of animal feed and animal-derived food using LC-MS/MS
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MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Mengmeng Feng,Huifang Ge,Ting Zhang,Jingbo Liu,Boqun Liu,Yali Yu
The quantification and analysis of free amino acids (FAAs) in serum is important for illness diagnosis due to its content varies with the body’s condition. In this study, a new sensitive analytical method based on liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS/MS) was optimized for simple and rapid simultaneous detection of 20 amino acids by pre-column derivatization. Amino acid derivatized by 9-fluorenyl methyl chloroformate (FMOC-Cl) were eluted and separated by simple mobile phase reagent in 20 min via gradient elution using a traditional reverse phase C18 column (150 × 4.6 mm, 5 μm), at the flow rate of 0.8 mL/min. After optimizing derivatization, LC-MS/MS conditions, and sample pre-treatment, this method was verified with LODs and LOQs ranging from 0.0237 to 0.2391 ng/mL and 0.079 to 0.7971 ng/mL. The intra- and inter-day precision was no more than 10 %. The overall accuracy and recovery varied from 88.4-111 % and 88.7–114 %, respectively. Those methods were first applied to mice serum with ulcerative colitis. The results showed that the levels of Ala, Arg, Trp, Lys, Cys, Tyr, and Phe significantly increased in pre-treated group by egg white peptides, which will participate in metabolism. This study provides a valuable reference for further research on the pathogenesis of ulcerous colitis and the development of functional foods to relieve inflammation and balance metabolism.
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FOOD CHEMISTRY
·
2025
·
IF 9.8
Luyue Zhao,Shu Li,Tong Wang,Sinan Wang,Jinhua Zhan,Jing Chen
Perfluorinated compounds are of extensive concern due to their prevalent use, persistence, and toxicities. There is a demand for extraction adsorbents that are efficient, easy to synthesize, and cost-effective. Herein, a magnetic nylon 6 nanocomposite (M-Ny6) was synthesized through a simple process and utilized as an adsorbent in magnetic solid-phase extraction (MSPE) of perfluorooctanoic acid (PFOA). The MSPE condition was optimized and the adsorption characteristics for PFOA was investigated. Based on the interaction between the amide groups on M-Ny6 and PFOA, the MSPE method was coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) for analyzing trace levels of PFOA in environmental water and bottled beverages. The established method demonstrated a detection limit of 1.2 ng L −1 with linear range across 50–800 ng L −1 and satisfactory recoveries (82.3–113.0 %) in spiked samples. The experimental results indicated that M-Ny6 is a promising and cost-effective MSPE adsorbent offering potential for large-scale applications in food analysis.
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MOLECULES
·
2024
·Vol. 29
·期 5
·1037
·
IF 4.2
Yujie Zhang,Jingjie Cao,Jiahan Su,Tingting He,Qianru Wang,Feng Wei,Xin Guo,Qibing Mei,Jing Zeng
Bitespiramycin, has been shown to have a therapeutic effect against respiratory tract inflammation, including a potential effect against COVID-19. A current clinical trial in China showed that bitespiramycin was an effective treatment for severe pneumonia and intracranial infection. However, there is lack of an analytical method to elucidate the distribution of bitespiramycin. In this study, a highly sensitive, rapid and reliable UPLC–MS/MS method was developed to comprehensively characterize the bitespiramycin distribution in various bio-samples, which is significantly improved upon the published work. A rapid sample preparation method was developed by usingn-butanol as the solvent to extract bitespiramycin from different bio-samples. The extract was then directly analyzed by UPLC–MS/MS coupled with an alkaline-resistant column after centrifugation which avoids the time-consuming concentration process under nitrogen and redissolution. The method was employed to accurately quantify bitespiramycin and its metabolites in rat plasma, tissues, and human cerebrospinal fluid. Notably, the presence of bitespiramycin and its metabolites was identified for the first time in various rat organs including brain, testis, bladder and prostate as well as in human cerebrospinal fluid. This newly developed approach shows great promise for drug distribution assays including other antibiotics and can help elucidate the ADME of bitespiramycin.
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ANALYTICAL CHEMISTRY
·
2022
·
IF 8.008
Hui-Yang Liao,Xuan Xiao,Rui Peng,Juan Le,Hai-Bo Wang,Shao-Ting Wang
Quantification of steroids possesses a crucial clinical value in early diagnosis and prognosis evaluation of various endocrine diseases. However, it is still challenging to realize feasible analysis of estrogens, androgens, progestogens, and corticoids within one single workflow. In this study, two derivatization reactions were newly designed for improvement: (1) acylation of phenolic hydroxyl on estrogens with isonicotinoyl chloride (INC) under the catalysis of 4-dimethylaminopyridine and (2) post-modification of oxime hydroxyl on hydroxylamine-pretreated ketosteroids with INC. Both reactions could conduct instantaneously at room temperature under aqueous conditions. Moreover, the resulting phenolic-INC and oxime-INC esters exhibited favorable MS responses. Through integrating these derivatization strategies with cold-induced phase separation technology, a feasible LC–MS/MS method was developed for simultaneous quantification of 15 multiclass steroids with proper sample consumption (50 μL serum), satisfying sensitivity (lower limit of quantitation at 0.01–5.00 ng/mL) and high throughput (40 min for sample-preparation). The practical applicability was tested by detecting 30 real samples from pregnant and non-pregnant women. The obtained results showed a good agreement with a previous validated methodology.
研究领域:
临床医学
·
分析化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2021
·
IF 3.205
Dan-Tong Zhao,Yi-Jun Gao,Wen-Jin Zhang,Tian-Chen Bi,Xiao Wang,Chun-Xia Ma,Rong Rong
Mycotoxins are poisonous secondary fungal toxic metabolites and harmful to human health. Traditional Chinese medicinal materials (TCMs), including more than two hundred functional foods, are vulnerably bred fungi, causing spoilage and multi-mycotoxins contamination. This study established a simultaneous analytical method by using multi-mycotoxins immunoaffinity column (multi-IAC) and HPLC-MS/MS to evaluate mycotoxins' contamination levels and natural incidence in TCMs. Aflatoxins (AFs, including AFB1, AFB2, AFG1 and AFG2), ochratoxin A (OTA), fumonisins (FB1 and FB2), zearalenone (ZEN), deoxynivalenol (DON) and T-2 toxins in three TCMs or functional foods of Polygalae Radix (PR), Coicis Semen (CS) and Eupolyphaga Steleophaga (ES) were detected. The systematically investigated results of 30 batch AFB1 positive samples revealed co-occurrence and correlation of multi-mycotoxins are significant differences in various matrices. All the samples in this study contain more than 5 mycotoxins. AFB1-AFs, AFB1-FBs, AFB1-DON, and AFB1-T-2 are the most observed co-occurrence, AFB1-OTA is also of concern due to its synergistic toxicity. This study's results can be used to establish guidelines for screening mycotoxin contaminants and limitations on acceptable levels in TCMs. Simultaneously, mycotoxin's correlation results in different matrices can also provide a reference for the standardization of TCM production and processing.
研究领域:
食品科学
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分析化学
·
毒理学
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Horticulturae
·
2025
·Vol. 11
·期 12
·1417
·
IF 3
Mingzheng Duan,Liuyuan Bao,Ting Jiang,Kangjian Song,Yubo Chen,Sijiu He,Xiande Duan,Muhammad Ikram,Shunqiang Yang,Muhammad Junaid Rao
Strawberry fruit quality is linked to its phytochemical composition, yet the diversity of non-volatile terpenoids remains largely unexplored. Therefore, a comparative LC-MS/MS-based metabolomic analysis of terpenoid profiles was conducted using three commercial cultivars (Fragaria×ananassa) and a wild accession ofFragaria nilgerrensis(HM). Results from this study showed that the HM cultivar had a total terpenoid abundance 5–6 times higher than the commercial cultivars. The HM cultivar was uniquely enriched in specific triterpenoids, such as 3β,6β,19α,24-Tetrahydroxyurs-12-en-28-oic acid and 13,27-Cyclo-2,3-Dihydroxy-11,19(29)-Ursadien-28-Oic Acid, which was over 450 times higher than the ‘Danxue’ and ‘Fenyu’ commercial strawberry cultivars. Conversely, sesquiterpenoids like Alismol and Pterocarpol were 100 times lower in HM than in the commercial cultivars. This enhanced triterpenoid accumulation strongly correlated with a superior capacity to scavenge free radicals in vitro, with HM showing maximum capacity, as measured by the DPPH assay. These findings highlight the value of wild strawberry germplasm as a reservoir of biochemical diversity for breeding strawberries with enhanced functional quality.
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Journal of Environmental Sciences
·
2024
·
IF 5.9
Shuang Chen,Yue Qiao,Youwei Jiang,Wei Qiu,Shuang Zang,Jing Zhang,Xianshi Wang,Jun Ma
Halogenated aromatic disinfection byproducts (DBPs) are gradually receiving attention due to their high detection frequency and usually higher toxicity than regulated DBPs. In this study, we established a solid phase extraction (SPE)-LC-MS/MS method to simultaneously trace analyze 59 halogenated aromatic DBPs. The limits of detection and limits of quantification of halogenated aromatic DBPs ranged from 0.03 ng/L to 135.23 ng/L and 0.1 ng/L to 450.76 ng/L, respectively. The range of recoveries and relative standard deviation (RSD) in river water were between 72.41 % to 119.54 % and 1.86 % to 16.03 %, respectively. Therefore, this method can be used to accurately analyze trace levels of halogenated aromatic DBPs in drinking water. The occurrence and transformation of halogenated aromatic DBPs were explored based on this method. In the chlorinated simulated source water and chlorinated river water, 20 and 45 halogenated aromatic DBPs were determined, respectively. The active halogen species (HOCl, HOBr, and HOI) first reacted with natural organic matter (NOM) to form halogenated aromatic DBPs. Then, chlorine further reacted with the halogenated aromatic DBPs to convert them into small-molecule halogenated aliphatic DBPs through oxidation, electrophilic substitution, and hydrolysis reaction, etc. In the chlorinated simulated source water, chlorinated river water, and tap water, the toxicity contribution of bromoacetic acids (Br-HAAs) accounted for the majority (> 71.16 %). Given that halogenated aromatic DBPs are intermediate products of halogenated aliphatic DBPs, controlling the formation of halogenated aromatic DBPs is beneficial in decreasing the formation of halogenated aliphatic DBPs, thereby diminishing the toxicity of drinking water.
研究领域:
环境科学
·
分析化学
·
公共卫生
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2026
·
IF 3.4
Yue Shi,Fangqi Cao,Xin Bai,Xia Ran,Xiaoliang Yuan,Daiwen Zhang,Zhiru Xu,Chaojun Li
Validated LC-MS/MS for 4-MEC, M1 and M2 in whole blood • Applied to IV and intragastric pharmacokinetic study • First in vivo PK characterization of 4-MEC and major metabolites • M2 shows prolonged exposure and extended detection window 4-Methyl- N -ethylcathinone (4-MEC) is a novel psychoactive substance and its in vivo exposure characterization remains unknown. In this study, a sensitive and robust liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and fully validated for the simultaneous quantification of 4-MEC and its two major metabolites in rat whole blood. Then it was applied to pharmacokinetic studies of 4-MEC in rats by intravenous and intragastric administration, characterizing the concentration-time profiles of the parent compound and its metabolites. The results revealed distinct exposure patterns between 4-MEC and its metabolites. Notably, M2 ( N -deethylated metabolite) exhibited a prolonged detection window compared with 4-MEC, supporting metabolite-based monitoring strategies and thereby extending its application in forensic toxicology and drug abuse identification.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Lili Liu,Yaping Huang,Qingqing Wang,Ziyuan Wang,Ke Pan,Jian Zhang,Ying Peng,Guangji Wang,Zhiqi Yin,Jianguo Sun
As a plant with a rich history of medicinal and dietary use, Gynostemma pentaphyllum (Thunb.) Makino is predominantly characterized by the gypenosides. Contemporary research has demonstrated that these saponins possess significant hypolipidemic and hypoglycemic effects. This study focused on developing an LC-MS/MS approach to elucidate the pharmacokinetic profiles of 13 gypenosides in rat models. The separation was accomplished using a ZORBAX Eclipse Plus C18 column (2.1 mm × 100 mm, 1.8 µm). Detection was facilitated by employing positive electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The analytical method was fully validated, including selectivity, linear response, measurement precision, analytical accuracy, extraction efficiency, matrix interference, and sample stability. The lower limit of quantification (LLOQ) for all compounds was 10 ng/mL, with each exhibiting a favorable linear relationship (r ≥ 0.9960). The precision, as measured by the relative standard deviation (RSD) for intra-day and inter-day variability, did not exceed 8.41 %. The accuracy, expressed as the relative error (RE), varied from −4.42–8.42 %. The recovery rate of the extraction process was between 92.02 % and 114.77 %, and no notable matrix effects were detected. The stability of the compounds was confirmed under four distinct storage conditions. Pharmacokinetic results indicated that all analytes displayed rapid absorption, prolonged retention, and slow elimination in rats, and exhibited nonlinear pharmacokinetics at low, medium, and high dosage levels. This study has established a quantification method for 13 gypenosides and successfully applied it to their pharmacokinetic studies in rats, providing a foundation for their further development and utilization.
研究领域:
中药学
·
分析化学
·
药理学
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