ANALYTICA CHIMICA ACTA
·
2026
·
IF 6.1
Keqiang Shi,Jiancong Liao,Cuirong Sun,Hongru Feng,Yuanjiang Pan
RNA modifications are vital for all living organisms. A total of at least 63 types of uridine modification have been discovered, accounting for the largest proportion of all reported RNA modifications. Uridine modifications have also been shown to be dysregulated in various human diseases. However, it's well known that mass spectrometry analysis of uridine modifications is limited by their low ionization efficiencies. Here, we developed a simple and robust method for the simultaneous identification and quantification of 22 uridine modifications in biological samples. In fact, uridine and lots of its modifications are more easily ionized in negative ion mode, compared with positive ion mode commonly used. Besides, the fragmentation patterns of uridine modifications in negative ion mode could provide more structural information, compared with well-known glycosidic bond cleavage in positive ion mode. Furthermore, simply by adding 0.2 mM acetic acid into the mobile phase, the peak areas of uridine and all 22 uridine modifications in negative ion mode could be improved by 4.1-55.4 folds. With this novel method, we quantified 16, 14, 10, 12 and 16 uridine modifications in 293T total RNA, 293T small RNA, E. coli tRNA, S. cerevisiae tRNA and wheat germ tRNA, accordingly. This study provides a general good method for researchers interested in the identification and quantification of uridine modifications in various biological samples.
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BIOMEDICAL CHROMATOGRAPHY
·
2017
·Vol. 31
·期 9
·e3962
·
IF 1.613
Yunsu Ma,Qianru Wang,Hongwen Zhang,Lijun Xie,Juan Chen,Mao Huang,Yun Liu,Yuanyuan Wang,Libin Wang,Luning Sun,Ning Ou
This study presents a high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) method for the simultaneous determination of antofloxacinin and its main metabolite – N -demethylated metabolite ( N- DM) – in human urine. Ornidazole was used as the internal standard. This was a clinical urine recovery study, in which 10 healthy Chinese volunteers were intravenously administered a single 200 mg dose of antofloxacin hydrochloride. Compounds were extracted by albumen precipitation, after which samples were isocratically eluted using a Poroshell 120 SB-C 18 column, and were analysed using HPLC–MS/MS under electronic spray ionization positive ion mode. The method was successfully applied in a urine pharmacokinetic study of antofloxacinin, with a detection range of 0.02/0.01 to 200/100 μg/mL (for antofioxacin/ N- DM).The average percentages of antofioxacin/ N- DM measured in urinary excretion frp, 10 volunteers were 54.9 ± 5.7/8.2 ± 2.5% in 120 h duration.
研究领域:
药物分析
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临床药理学
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分析化学
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药代动力学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Qiao Deng,Jianliang Li,Jingjing Xu,Xiaojing Zhao,Dan Wei,Xu Wang
The accurate quantification of urinary modified nucleosides, promising non-invasive cancer biomarkers, is hindered by their trace concentrations and complex matrix interference. To overcome this challenge, we developed the facile synthesis of a novel ternary magnetic composite (MCS-100GO) by integrating chitosan (CS) and graphene oxide (GO) onto the magnetic core, utilized as adsorbent for magnetic solid-phase extraction (MSPE). The adsorbent leverages the combined effects of hydrogen bonding (from CS and GO) and π-π interactions (from GO) for highly efficient capture, while the magnetic core enables rapid and simple separation. Systematic optimization demonstrated exceptional performance for 3-methylcytidine (m 3 C) and 7-methylguanosine (m 7 G). The MCS-100GO composite achieved rapid adsorption equilibrium (3 min), high maximum adsorption capacities (0.7730 mg/g for m 3 C and 0.7561 mg/g for m 7 G). The developed MCS-100GO based MSPE-HPLC-MS/MS method, validated according to FDA guidelines, exhibited excellent sensitivity (LODs: 0.015–0.030 μg/L), a wide linear range (0.050–50 μg/L; R 2 > 0.9995), and high precision (RSD < 6.4 %). Furthermore, parallelism experiments with a coefficient of variation (CV) of 9.7 % confirmed no significant matrix effects. Compared to existing methods, this approach offers a superior balance of low adsorbent dosage, sensitivity, speed, presenting a promising and efficient strategy for high-throughput analysis of urinary nucleoside biomarkers.
研究领域:
分析化学
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生物材料
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癌症生物标志物
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代谢组学
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环境与生物医学分析
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ECOTOXICOLOGY AND ENVIRONMENTAL SAFETY
·
2020
·
IF 4.872
Yue Su,Weijun Wang,Jiye Hu,Xiaolu Liu
The dissipation and residues of tembotrione in corn field application were investigated using liquid chromatography tandem mass spectrometry (LC-MS/MS) method. The average recoveries of tembotrione in maize, corncob, and straw were in the ranges of 98–107% with relative standard deviations (RSDs ≤9.3%), respectively. The recoveries of M5 was in the ranges of 90–108% in all three matrices of maize, with RSDs were 3.3–12.8%. The LODs for tembotrione and M5 in maize were 0.85 μg/L and 1.0 μg/L, 0.84 μg/L and 0.43 μg/L in corncob, 0.94 μg/L and 1.5 μg/L in straw, respectively. The LOQs of the method in maize grain, corncob and straw were 0.01, 0.01 and 0.05 mg/kg for both analytes, respectively. The dissipation of tembotrione in straw was in compliance with the first-order dynamic equation, with half-lives of 1.18–1.23 days at Beijing and Heilongjiang. Total residue of tembotrione in maize grain and corncob matrix were both below 0.02 mg/kg, lower than the max residue limit (MRL) recommended by european food safety authority (EFSA). Risk quotients (RQs) of this pesticide was assessed via comparing national estimated daily intake with acceptable daily intake . The dietary intake risk of tembotrione residue in maize was very low for all groups of Chinese residents. These data could provide scientific data and strategies and facilitate Chinese government to establish the MRLs of tembotrione.
研究领域:
农业化学
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环境科学
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食品安全
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分析化学
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ENVIRONMENTAL RESEARCH
·
2023
·
IF 8.3
Hao Cui,Wei Zhan,Xuan Ji,Mingye Jiang,Xiaoting Wu,Minru Huang,Chenhui Huang,Shanshan Ma
With the widespread use of sulfonamide antibiotics (SAs), SAs are detected as residues in aquatic environments, posing a serious threat to human life and safety. Because of their high water solubility, fast transmission rate, and strong antibacterial properties, the safe disposal of SAs has become a key constraint for water quality assurance. Therefore, an ultrasound (US)-assisted zero-valent iron (ZVI)/persulfate (PS) system was proposed to explore the rapid and effective degradation of SAs. Comparative experiments were performed to study the removal of sulfadiazine (SDZ) by US, ZVI, PS, US/ZVI, US/PS, ZVI/PS, and US-ZVI/PS systems, respectively. Experimental results indicated that the highest removal efficiency of SDZ was ahieved in US-ZVI/PS system (97.4%), which were 2–44 times higher than that in other systems. Furthermore, the degradation efficiency of five typical SAs was achieved over 95%, demonstrating the effectiveness of the US ZVI/PS system for SAs removal. Also, quantum chemical computations for potential reactive sites of SAs and intermediate product detection by HPLC‒MS/MS were performed. The radical attack on active sites of SAs, such as N atom (number 7), was the main reason for SAs removal in US-ZVI/PS system. Besides, the common degradation pathways of six typical SAs were defined as S–N bond cleavage, C–N bond cleavage, benzene ring hydroxylation, aniline oxidation, and R substituent oxidation. Interestingly, the unique pathway of “SO 2 group extraction” was observed in the degradation of six-membered ring SAs. Therefore, the US-ZVI/PS system is a promising and cost-effective method for the removal of SAs and other refractory pollutants.
研究领域:
环境科学
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化学工程
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水处理
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高级氧化过程
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TALANTA
·
2026
·
IF 6.7
Haoran Li,Shijun Xiong,Beibei Chen,Zhekuan Wu,Zhen Zhou,Yong Liang,Man He,Bin Hu
Amadori and Heyns compounds are key Maillard reaction intermediates, resulting from the reaction of a certain amino acid with glucose (Glu) or fructose (Fru), respectively. They play a dual role in augmenting cigarette aroma and attenuating sensory irritation, and their quantification in tobacco is vital for tobacco quality evaluation and Maillard reaction mechanism study. Currently, simultaneous quantification of Amadori and Heyns compounds derived from the same amino acid, which present as isomers, is encumbered by poor chromatographic separation, and reliance on unavailable specific fragment ions. Herein, a method based on high performance liquid chromatography combined with tandem mass spectrometry (HPLC-MS/MS) detection was developed for the simultaneous quantification of Amadori and Heyns compounds derived from the same three amino acid (alanine, proline, phenylalanine, abbreviated as Ala, Pro, and Phe, respectively) with an ion ratio strategy. Under the optimized conditions, the limits of detection ranging from 2.22 to 6.94 ng/mL were obtained for six target analytes (Fru-Phe/Glu-Phe, Fru-Pro/Glu-Pro, Fru-Ala/Glu-Ala). When the method was applied to tobacco leaf powder extracts, target Amadori and Heyns compounds were found in the range of 0.65-56.4 μg/g, with Heyns compounds consistently less abundant than Amadori counterparts. In the recovery test, target analytes showed recoveries of 76.8-111%. Compared with reported methods, the proposed method features universal applicability without requiring characteristic fragment ions or chromatographic separation. It provides a reliable tool for analyzing hard-to-separate sugar-derived Maillard intermediates in tobacco.
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JOURNAL OF SEPARATION SCIENCE
·
2026
·Vol. 49
·期 5
·e70448
·
IF 3.6
Tao Pei,Xueyun Wang,Jiye Hu
To control thrips in eggplant cultivation, a new pesticide formulation (9% emamectin benzoate·spinetoram microemulsion) is under registration in China. However, the residues of emamectin benzoate (EMB), spinetoram, and prime metabolites of spinetoram in eggplant remained unclear. In this study, field trials were performed in accordance with good agricultural practice across eight provinces of China. The pesticide formulation was sprayed once at 13.5 g a.i./ha, and the recommended pre-harvest interval was 7 days. For the simultaneous determination of EMB, spinetoram, and its metabolites in eggplant, a modified quick, easy, cheap, effective, rugged, and safe method combined with high-performance liquid chromatography tandem mass spectrometry was developed and validated. The combination of 25 mg of primary-secondary amine, 25 mg of Nano-ZrO 2 , and 5 mg of multi-walled carbon nanotubes was applied to purify the eggplant extracts. Method validation demonstrated excellent linearity ( r ≥ 0.9991), acceptable accuracy with recoveries of 82.7%–102.6%, precision (relative standard deviations ≤7.7%), sensitivity (limits of detection, 6.59 × 10 −5 –3.06 × 10 −3 ng; limits of quantification, 0.0025–0.01 mg/kg), and matrix effects (≤25.2%). When harvested after the recommended 7-day interval, the residues of EMB (<0.01 mg/kg) and spinetoram (≤0.025 mg/kg) in eggplant were lower than the maximum residue limits in China. The residues of metabolites N- formyl-XDE-175-J and N- demethyl-XDE-175-J in eggplant were lower than the limits of quantification (0.01 mg/kg). This study offers recommendations for the effective use of this pesticide formulation on eggplant.
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JOURNAL OF INTERNATIONAL MEDICAL RESEARCH
·
2020
·
IF 1.287
Yulong Gu,Xianglan Piao,Dan Zhu
ObjectiveThis study aimed to develop and validate a high-performance liquid chromatography–tandem mass spectrometry method to simultaneously determine three bioactive components of the Huangqi Chifeng decoction (HQCF) in rat plasma.MethodsTaxol was used as an internal standard in the developed method. Chromatographic separation was performed on a C18 column using a gradient elution with 0.1% formic acid in acetonitrile (v/v) and 0.1% formic acid in water (v/v) as the mobile phases at a flow rate of 0.4 mL·minute−1. All compounds were monitored via selected reaction monitoring with an electrospray ionization source.ResultsThe lower limits of quantification of paeoniflorin, calycosin, and prim-O-glucosylcimifugin were 15.0, 0.75, and 0.75 ng·mL−1, respectively. The calibration curves indicated optimal linearity (r > 0.99) across the concentration ranges. The specificity, precision, accuracy, recovery, matrix effect, and stability of the method were validated. This method was successfully applied in a pharmacokinetics study of the three compounds in rat plasma.ConclusionThe pharmacokinetics results provide insights into the mechanisms of HQCF in vivo and its future clinical application.
研究领域:
中药学
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分析化学
·
药理学
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PHARMACEUTICAL BIOLOGY
·
2021
·
IF 3.503
Cai-Yun Zhang,Ya-Ting Lu,Yin-Feng Tan,Qi-Bing Liu,Lin Dong,Ning Ma,Wei-Ying Lu,Zhi-Heng Su,Xiao-Po Zhang
Context Tadehaginoside, an active ingredient isolated from Tadehagi triquetrum (Linn.) Ohashi (Leguminosae), exhibited various biological activities. However, the pharmacokinetics and tissue distribution which affect tadehaginoside’s therapeutic actions and application remain elusive.Objective To clarify the metabolism of tadehaginoside in vivo.Materials and methods The pharmacokinetics and tissue distribution of tadehaginoside and its metabolite p-hydroxycinnamic acid (HYD) were investigated using LC-MS/MS. Pharmacokinetic parameters were determined in 10 Sprague-Dawley rats divided into two groups, the intravenous group (5 mg/kg) and the oral group (25 mg/kg). For the tissue-distribution study, 20 rats were intravenously given tadehaginoside (5 mg/kg) before the experiment (n = 4). Biological samples were collected before drug administration (control group) and after drug administration.Results The linearity, accuracy, precision, stability, recovery and matrix effect of the method were well-validated and the results satisfied the requirements of biological sample measurement. Treatment with tadehaginoside via intragastric and intravenous administration, the calculated Cmax in rats was 6.01 ± 2.14 ng/mL and 109.77 ± 4.29 ng/mL, and Tmax was 0.025 ± 0.08 h and 0.08 h, respectively. The results indicated that the quick absorption of tadehaginoside was observed following intravenous administration, and tadehaginoside in plasma of rats with intragastric administration showed relatively low concentration may be due to the formation of its metabolite. Tissue-distribution study indicated that kidney and spleen were the major distribution organs for tadehaginoside in rats and there was no long-term accumulation in most tissues.Discussion and conclusion These results could provide clues for exploring the bioactivity of tadehaginoside based on its pharmacokinetic characteristics.
研究领域:
药理学
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分析化学
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MOLECULES
·
2022
·Vol. 27
·期 21
·7636
·
IF 4.927
Xuyan Fan,Tao Tang,Song Du,Ningning Sang,Hao Huang,Chenghui Zhang,Xueping Zhao
A rapid, efficient, simple, and high-throughput method for the simultaneous determination of 108 pesticide residues in three traditional Chinese medicines (TCMs) was established, comprising an improved QuEChERS method in combination with HPLC-MS/MS based on mixed samples. A quantity of 10 mL of acetonitrile was used as extraction solvent, and 10 mg of amino-modified multi-walled carbon nanotubes (MWCNTs-NH2) and 150 mg of anhydrous magnesium sulfate (MgSO4) were selected as sorbents for dispersive solid phase extraction. The performance of the method was verified according to the analytical quality control standards of SANTE/11813/2017 guidelines. With good linearity (R2> 0.9984) in the range of 2–200 μg/L for all pesticides in the selected matrices, and good accuracy, precision, and high sensitivity, the recoveries were in the range of 70–120% for more than 95% of the pesticides, with a relative standard deviation (RSD) of less than 16.82% for all. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.01–3.87 μg/kg and 0.07–12.90 μg/kg, respectively, forFritillaria thunbergiiMiq (F. thunbergii),Chrysanthemum MorifoliumRamat (C. morifolium), andDendrobium officinaleKimura et Migo (D. officinale). The method was successfully applied to 60 batches of actual samples from different regions.Keywords:pesticide residue;QuEChERS;MWCNTs-NH2;traditional Chinese medicines
研究领域:
分析化学
·
药学
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FOOD CHEMISTRY
·
2025
·
IF 9.8
Huiyu He,Rui Wang,Rongbin Nie,Nan Dong
Pretreatment technology suffers from drawbacks such as tedious operation, low efficiency, and poor selectivity. Hence, we presented a singly capped cucurbit[7]uril-mediated magnetic solid phase extraction (Q[7]-MagSPE) combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for multiresidue analysis of 20 pesticides. The Q[7]-MagSPE was constructed by assembling Q[7] onto the gold magnetic nanoparticles (GoldMag) via the reaction between one of the electron-rich carbonyl portals of Q[7] and gold. The host-guest interaction activity of supramolecules, the high dispersibility and easy separability of GoldMag were integrated in the Q[7]-MagSPE. The detection limits for 20 pesticides were lower than 10.3 ng/kg, and the recoveries were 71.55 – 110. 6 % . Moreover, the reusability of the Q[7]-GoldMag and effect of washing times on the pesticide residue were evaluated to be satisfactory. Therefore, the Q[7]-MagSPE provides a rapid and robust pretreatment method for the multiresidue determination of pesticides in vegetables, which is of great significance for food safety.
研究领域:
分析化学
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食品安全
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纳米技术
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农药分析
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超分子化学
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高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2026
·Vol. 40
·期 3
·e70366
·
IF 1.7
Zhiyuan Li,Qing Shao,Hongqun Qiao
A sensitive and robust HPLC-MS/MS method was developed and validated for the simultaneous determination of YWS22026 and its major metabolite M3 in rat plasma using protein precipitation. Chromatographic separation was achieved on a Shim-pack Scepter C18 column (4.6 × 50 mm, 3 μm) with a gradient elution program (mobile phase A: 0.2% formic acid in water; mobile phase B: methanol) at a flow rate of 0.9 mL/min. Detection was performed via positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode. The method demonstrated excellent specificity, accuracy (relative error, %RE < 9.1%), precision (relative standard deviation, %RSD < 9.9%), and linearity (5–2000 ng/mL for both analytes). The lower limit of quantification (LLOQ) was 5 ng/mL. Stability studies confirmed that plasma samples remained stable under various storage conditions (at room temperature for 10 h, −20°C for 22 days, three freeze–thaw cycles, and 4°C autosampler storage for 73 h). This validated method was successfully applied to a 26-week concomitant toxicokinetic study in Sprague–Dawley rats, which revealed significant sex-related differences in exposure for both YWS22026 and M3. These findings provide valuable insights for informing the safety assessment of YWS22026 in subsequent clinical trials.
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