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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PubMed
高影响因子
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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高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2026
·
IF 3.8
Wang Dong,Li Mengrong,Zhang Xiangyu,Chai Shiwei,Chen Di
A novel ultrasound-assisted magnetic sorbent–wrapped stick dip extraction (UA-MSWS-DE) method was developed for the batch-scale determination of seven tyrosine kinase inhibitors (TKIs) in human plasma. The extraction device was fabricated by immobilizing octadecylphosphonic acid–functionalized magnetic nanoparticles onto flame-sealed glass capillaries embedded with magnets. Ultrasonic-assisted dip extraction was used to extract TKIs from diluted plasma, followed by quantification via liquid chromatography–tandem mass spectrometry (LC-MS/MS). Key extraction parameters were systematically optimized, yielding the following optimal conditions: sample pH 5.0 and volume 1.0 mL, sorbent particle size 20 nm and dosage 10 mg, extraction time 20 min, and desorption with 150 µL of ethanol for 8 min. The method demonstrated excellent linearity ( R 2 ≥ 0.99), low limits of quantification (0.1–5.0 ng/mL), and good intra-/inter-day precision (RSDs < 14.95%). The accuracy in blinded plasma samples, tested at 0.25–25% of the studied concentration range, ranged from 87.13 to 112.33%. Compared to conventional magnetic dispersive solid-phase extraction, the UA-MSWS-DE strategy simplifies handling and is designed to facilitate potential parallel processing using only an ultrasonic bath. Five greenness metrics confirmed the method’s high sustainability. Furthermore, the modular design enables adaptation to other analytes by modifying the sorbent coating, making UA-MSWS-DE a sensitive, green, and automation-ready method for therapeutic drug monitoring. Graphical
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 12
·e4373
·
IF 1.688
Qi Wen,Hai-Long Li,Feng Chen,Jing-Wen Gong,Wei-Wei Guan,Nai-Guang Fu,Yin-Feng Tan
The aim of the present study was to develop a rapid, specific and sensitive LC–MS/MS method for the determination of DPHB [7-(4″-hydroxy-3″-methoxyphenyl)-1-phenyl-4-hepten-3-one] in rat plasma using yakuchinone A as an internal standard (IS). n -Hexane was used for the extraction of DPHB from rat plasma. Chromatographic separation of DPHB was achieved using a Kinetex XB-C 18 column (2.10 × 50 mm, 2.6 μm) at 40°C. The mobile phase consisted of water (containing 0.1‰ formic acid, A) and acetonitrile (containing 0.1‰ formic acid, B) under a gradient elution at a flow rate of 0.3 mL min −1 . Positive electrospray ionization and multiple reaction monitoring mode were used for detection. The selected precursor ion to product ion pairs, m / z 311.3 → 137.0 for DPHB and m / z 313.1 → 137.0 for yakuchinone A, were monitored. Good linearity was observed over the concentration range from 2 to 2000 ng mL −1 ( r = 0.9969). The recovery efficiency of DPHB from rat plasma was 54.8–69.7%, while the matrix effect ranged from 99.7 to 113%. Intra- and inter-day precision and accuracy values were within ±15% at three different quality control concentration levels. This validated method was successfully applied to pharmacokinetic studies in rats after a single p.o. or i.v. dose of DPHB solution. The route of administration significantly influenced systemic exposure to DPHB, and low bioavailability of DPHB was observed. The method developed here will be further improved and used in future pharmacokinetic studies.
研究领域:
分析化学
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药学
·
药代动力学
·
生物分析
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DOI
高影响因子
FOOD CHEMISTRY
·
2026
·
IF 10.4
Xia Xu,Chen Liang,Zengbo Fang,Ting Zhao,Mingjie Liu,Yan Cui
A novel chiral derivatization reagent {DMT-OTZD-3( S )-Apy} was synthesized. • A sensitive LC-MS/MS method was developed for the simultaneous determination of six NSAID enantiomers. • Determination of NSAID enantiomers was carried out firstly in multi-specie meat products. In stock farming, illegal use of non-steroidal anti-inflammatory drugs has caused food safety problems. A novel chiral derivatization reagent targeted carboxyl groups, ( S )-[(( R )-1-(4,6-dimethoxy-1,3,5-triazine-2-yl)-2-oxothiazolidine-4‑carbonyl] pyroli-dine-3-amine {DMT-OTZD-3( S )-Apy}, was synthesized. After derivatization with it, the first multi-residue and simultaneous determination targeted six NSAID enantiomers in beef and mutton products was conducted. The method was validated to be selective, and got an excellent linear relationship for all enantiomers within their respective concentration ranges ( r 2 ≥ 0.9990). The average recoveries were from 91.7% to 104.3%, and the RSDs corresponding to intra-day and inter-day precision did not exceed 6.2%. The limit of detections spanned the interval of 0.30–1.42 ng/g, which were far lower than maximum residue limits established by China and the European Union. The method would provide methodology support for the risk assessment of NSAIDs in meat products from enantiomeric levels. Download: Download high-res image (122KB) Download: Download full-size image
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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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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高影响因子
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
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分析化学
·
药理学
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高影响因子
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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高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Ziyuan Zheng,Wenguang Yan,Wenlong Liu,Zihao Cai,Yanjun Ding,Jiang Ling
Volatile organic compounds (VOCs) play a critical role in human physiology, with their concentrations serving as key indicators of physiological states. Among these, trans-4,5-epoxy-(E)-2-decenal, a volatile organic compound found in mammalian blood, exhibits unique chemical reactivity and olfactory sensitivity due to its molecular structure, which is closely associated with lipid peroxidation processes. However, conventional detection methods, such as gas chromatography-olfactometry-mass spectrometry (GC-O-MS), suffer from limitations including inherent subjectivity, poor reproducibility, stringent operational requirements, and low throughput, which undermine their clinical reliability. To address these challenges, this study developed an optimized liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for accurate qualitative and quantitative analysis. Given the poor detectability of aldehydes via LC-MS/MS, 2,4-dinitrophenylhydrazine (DNPH) derivatization was employed to enhance the chromatographic behavior and retention of the target compound. Additionally, HLB solid-phase extraction (SPE) columns was employed for purification to enhance the sensitivity of LC-MS/MS for the detection of trans-4,5-epoxy-(E)-2-decenal. Following derivatization, trans-4,5-epoxy-(E)-2-decenal demonstrated strong retention during chromatographic separation. The mobile phase, composed of acetonitrile and ultrapure water, exhibited significantly superior performance compared to combinations of acetonitrile with ammonium acetate buffer. Under optimized conditions, the LC-MS/MS method demonstrated excellent linearity for trans-4,5-epoxy-(E)-2-decenal within a range of 1–300 ng/mL, with correlation coefficient (R 2 ) of 0.9984, detection limit (LOD) of 0.3 ng/mL. The relative standard deviation (RSD) for spiked blood samples in the experiment was 12.53 %.
研究领域:
分析化学
·
生物化学
·
医学诊断
·
代谢组学
·
质谱分析
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高影响因子
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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高影响因子
FOOD AND AGRICULTURAL IMMUNOLOGY
·
2021
·
IF 3.101
Jie-Biao Guo,Tai-Long Wei,Qing-Hua He,Jin-Sheng Cheng,Xiu-Zhen Qiu,Wang-Pei Liu,Xian-Quan Lan,Lu-Fen Chen,Min Guo
A magnetic separation-based immunosensor for deoxynivalenol assay, coupled with a nano-affinity cleaning up for instrumental confirmation, was developed. Maltose-binding protein with mimic epitope of DON was coupled to CdSe/ZnS quantum dot nanobeads for fluorescent reporter. Graphene oxide was linked with magnetic nanoparticles and protein G for immunomagnetic adsorbent. The magnetic separation of reporter could be inhibited by DON so the fluorescent remained in the solution indicates a good quantitative correlation to DON concentration. The DON separated by immune adsorbent can be cleaned up for instrumental confirmation. The optimized immunosensor showed results as follows: the linear range was in 0.3–3000 ng mL−1. The limits of detection (S/N = 3) were 0.50, 1.0, and 3.0 ng mL−1 in different backgrounds. The recoveries for DON-spiked samples range from 78.7% to 88.5%. Both results of UPLC-MS/MS based on affinity column purification and coupled with nano-affinity cleaning up showed a good agreement with the current immunosensor.
研究领域:
食品安全检测
·
免疫学
·
分析化学
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高影响因子
Drug Research
·
2020
·Vol. 70
·期 11
·528-540
·
IF 0
Yuxin Zhang,Yihua Lu,Lijuan Wang,Yuan Tian,Zunjian Zhang
Loratadine (LOR) and its major metabolite, desloratadine (DL) are new-generation antihistamines. The hydroxylated metabolites of them, 6-OH-DL, 5-OH-DL and 3-OH-DL are also active because of their ability to inhibit binding of pyrilamine to brain H1 receptors and a tendency for distributing to specific immune-regulatory tissues. In this study, a new validated LC-MS/MS method to simultaneously quantify LOR, DL, 6-OH-DL, 5-OH-DL and 3-OH-DL in plasma and tissues was established and applied to an investigation of their pharmacokinetics and target-tissue distribution tendency for the first time. Pharmacokinetics parameters in rat were measured and the results suggest that the body’s exposure to active metabolites were much higher than to the prodrug with LOR, but much lower with DL. The tissue distribution study shows that LOR, DL and their active metabolites were widely distributed in the liver, spleen, thymus, heart, adrenal glands and pituitary gland. For immune-regulatory tissues, the concentrations of LOR, DL and their active metabolites in the spleen were much higher than in the thymus, which is related to the spleen, one of the sites where immune responses occur. LOR and its metabolites might inhibit immune-mediated allergic inflammation through the hypothalamic-pituitary-adrenal (HPA) axis. It was also found that the concentration of LOR in the heart was highest after liver and adrenal glands while those of DL, 6-OH-DL and 5-OH-DL in the liver, adrenal glands and spleen were all higher than those in the heart, which suggests that LOR may have a greater tendency to distribute in the heart than its metabolites.
研究领域:
药理学
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分析化学
·
免疫学
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