MOLECULES
·
2021
·Vol. 26
·期 11
·3344
·
IF 4.412
Shunyu Yao,Zixi Zhao,Wang Lu,Xin Dong,Jiye Hu,Xiaolu Liu
The chemical fungicide fludioxonil is widely used to control post-harvest fungal disease in cherries. This study was implemented to investigate the dissipation behaviours and residues of fludioxonil on cherries. A reliable and efficient analytical method was established. Cherry samples from four product areas were analyzed by QuEChERS and HPLC-MS/MS methods with acceptable linearity (R2> 0.99), accuracy (recoveries of 81–94%), and precision (relative standard deviation of 2.5–11.9%). The limits of quantification (LOQs) and limits of detection (LODs) of cherries were 0.01 mg/kg and 0.005 mg/kg. The dissipation of fludioxonil on cherries followed first order kinetics with half-lives of 33.7–44.7 days. The terminal residues of fludioxonil were all lower than 5.00 mg/kg, which is the MRL recommended by the European Commission. According to Chinese dietary patterns and terminal residue distributions, the risk quotient (RQs) of fludioxonil was 0.61%, revealing that the evaluated cherries exhibited an acceptably low dietary risk to consumers.Keywords:fludioxonil;cherry;HPLC-MS/MS;dissipation behaviour;residues;dietary risk assessment
研究领域:
食品科学
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农业化学
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毒理学
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产品关联
DOI
PubMed
高影响因子
Foods
·
2022
·Vol. 11
·期 13
·1843
·
IF 5.561
Lanlan Wei,Yanan Chen,Dongliang Shao,Jingjun Li
In this study, a packed-fiber solid-phase extraction (PFSPE)-based method was developed to simultaneously detect nine quinolones, including enrofloxacin (ENR), ciprofloxacin (CIP), ofloxacin (OFL), pefloxacin (PEF), lomefloxacin (LOM), norfloxacin (NOR), sarafloxacin (SAR), danofloxacin (DAN), and difloxacin (DIF), in pure milk, using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). Polystyrene (PS) and polyacrylonitrile (PAN) were combined to form PS-PAN composite nanofibers through electrospinning. The nanofibers were used to prepare the home-made extraction columns, and the process was optimized and validated using blank pure milk. The analytical method showed high accuracy, and the recoveries were 88.68–97.63%. Intra-day and inter-day relative standard deviations were in the ranges of 1.11–6.77% and 2.26–7.17%, respectively. In addition, the developed method showed good linearity (R2≥ 0.995) and low method quantification limits for the nine quinolones (between 1.0–100 ng/mL) for all samples studied. The nine quinolones in the complex matrix were directly extracted using 4.0 mg of PS-PAN composite nanofibers as a sorbent and completely eluted in 100 μL elution solvent. Therefore, the developed PFSPE-HPLC-MS/MS is a sensitive and cost-effective technique that can effectively detect and control nine quinolones in dairy products.Keywords:polystyrene-polyacrylonitrile nanofibers;quinolones;packed-fiber solid-phase extraction;HPLC-MS/MS;pure liquid milk
研究领域:
分析化学
·
食品科学
·
纳米技术
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Dan Wei,Ao Pan,Can Zhang,Ming Guo,Chaoyan Lou,Ju Zhang,Huizhen Wu,Xu Wang
A simple, rapid and sensitive vortex-assisted magnetic solid phase extraction (MSPE) method using core–shell structured magnetic covalent organic frameworks (Fe 3 O 4 /COF-TpBD) as adsorbents was established for simultaneous determination of aflatoxins, ochratoxins and enniatins in maize before high-performance chromatography tandem spectrometry detection. Fe 3 O 4 /COF-TpBD was facilely fabricated, characterized, and applied for simultaneous extraction of ten mycotoxins from maize. Key parameters affecting MSPE efficiency were investigated. The method possessed good linearity (0.05–50 μg/kg), high sensitivity (0.02–1.67 µg/kg for limits of detection), and satisfactory recoveries (73.8–105.3 %), with relative standard deviations less than 8.5 %. The amount of adsorbent used (5 mg) and the time required (0.5 min each for adsorption and for desorption) for MSPE were greatly shortened in comparison with the previous reports. Therefore, the fabricated Fe 3 O 4 /COF-TpBD exhibited a great potential for rapid extraction of common mycotoxins in maize, which can be attributed to its multiple interactions with the target mycotoxins.
研究领域:
分析化学
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食品安全
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真菌毒素分析
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产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2024
·
IF 5.7
Yan Liu,Jiajia Han,Guosheng Chen,Siming Huang,Shuyao Huang,Juan Zheng,Jianqiao Xu,Fang Zhu,Gangfeng Ouyang
Phytohormones are a class of endogenous substances that separately or synergistically regulate the growth, development, and differentiation of plants. Accurately and efficiently detecting and monitoring the concentration of plant hormones in living plants is of significant importance. Herein, a novel mesoporous carbon hollow spheres (MCHS)-based in vivo solid phase microextraction (SPME) probe was designed for in vivo sampling of plant hormones. The designed MCHS features the advantages of high surface area, porous shells, and large hollow spaces, facilitating the dynamic adsorption and enrichment of target phytohormone. In addition, a cationic polyelectrolyte, (poly (diallyl dimethyl ammonium chloride) (PDDA), was further modified onto the MCHS to expedite the extraction process by electrostatic interaction. Utilizing the MCHS@PDDA probe in combination with HPLC-MS/MS facilitated the continuous monitoring of three plant hormones (abscisic acid (ABA), indole-3-acetic acid (IAA), and gibberellin (GA3)) in Chinese aloe. The detection limit of this method was 0.016–0.090 μg/L, the linear range was 10–1000 μg/L, and both the RSD of the single probe (n = 6) and probe-to-probe test (n = 6) were less than 7.2 %. This method had excellent accuracy and good reproducibility comparable to the traditional sample pretreatment method. Ultimately, this established in-vivo SPME method was successfully adopted to quantify three selected plant hormones in living Chinese Aloes, providing a new method for the long-term monitoring of endogenous active substances in living system.
研究领域:
分析化学
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植物科学
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生物技术
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产品关联
DOI
PubMed
高影响因子
TALANTA
·
2022
·
IF 6.556
Ting Zhou,Guangzhao He,Changjia Hu,Kang Wu,Ying Liu,Jianguo Li,Anping Deng
5-Fluorouracil (5-FU) is an effective anticancer drug widely used in cancer treatment. In this study, two 5-FU derivatives containing a spacer arm with the carboxylic group at the end were synthesized, which were linked to the carrier proteins to form 5-FU-protein conjugates used as the immunogens for the production of monoclonal antibody (mAb). Based on the produced mAb, the highly sensitive and specific enzyme-linked immunosorbent assay (ELISA) for 5-FU detection was established. The IC 50 and LOD values of the assay were found to be 19.5 ng mL −1 and 0.5 ng mL −1 , respectively. There was no cross-reactivity (CR) of the ELISA with cytosine , thymine and uracil , which avoided the interference from inherent pyrimidines. The CR values of the assay with three substitutes of 5-FU (tegafur, 5-fluoro-2′-deoxyuridine, carmofur) were within 9.7%–17.6%. The produced mAb was also applied in sample extraction. The immuno-affinity column capable specific capturing 5-FU was prepared by immobilizing the mAb on Sepharose-4B gel and filling into a SPE column. The recoveries of 5-FU in spiked samples measured by ELISA were 72.4%–90.7% with RSD of 3.6%–8.3%. Five blood samples collected from patients were extracted by immuno-affinity column, then measured by ELISA and confirmed by HPLC-MS/MS. There was a good correlation between HPLC-MS/MS and ELISA. It is demonstrated that the developed ELISA combined with immuno-affinity extraction can be a powerful alternative method for the detection of 5-FU in blood samples.
研究领域:
药理学
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分析化学
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免疫学
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临床化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2024
·
IF 2.8
Qian Li,Yongfu Zeng,Lianfeng Ai,Maolin Wei,Xiaomeng Liu,Xiaochan Zhao,Haoran Zhang,Xiujuan Guo
A stable isotope dilution-liquid chromatography tandem mass spectrometry method based on a low-temperature derivatization strategy with 3-nitrophenylhydrazine (3-NPH) was developed for the determination of six volatile fatty acids (VFAs) in serum, urine, and feces. Ice acetonitrile was used to precipitate proteins and extract the target analytes. The extract was derivatized with 3-NPH methanol solution at 4 °C. BEH C8 (1.7 μm, 2.1 × 100 mm) column was used for chromatographic separation, and acetonitrile–water (both containing 0.01 % formic acid) were used as the mobile phase with a gradient elution of 10 min. Electrospray ionization source (ESI) in negative ion multiple reaction monitoring (MRM) mode were used for analyte detection. The regression coefficients R 2 of the calibration curves for the six VFAs were in the range of 0.9963–0.9994, and the LOQs were in the range of 0.02–0.5 μg mL −1 , with the recoveries in the range of 85.3–104.3 %, and the intra- and inter-day precision in the range of 1.8–9.1 %. The method is simple, accurate and reliable, and has been applied in the sensitive determination of VFAs in complex biological samples.
研究领域:
分析化学
·
生物医学
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DOI
PubMed
高影响因子
JOURNAL OF ENVIRONMENTAL SCIENCE AND HEALTH PART B-PESTICIDES FOOD CONTAMINANTS AND AGRICULTURAL WASTES
·
2021
·
IF 1.99
Zhongbei Zhang,Kai Ding,Zhou Lu,Nan Fang,Bo Wang,Zhiguang Hou,Zhongbin Lu
In the present study, an analytical method that combined a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method and high-performance liquid chromatography coupled with tandem mass spectrometry was developed to determine trifluorocide in fresh and dried ginseng roots, plants (stems and leaves), and soil. At three spiked levels (0.01, 0.1, and 1.0 mg kg−1), the mean recoveries (n = 15) of trifluorocide from fresh and dried ginseng roots, plants, and soil were in the range of 95.6 − 109.7%, with relative standard deviations less than 10.0%. The limits of quantitation of different matrices were determined to be 0.01 mg kg−1. Dissipation and residue study of trifluorocide was conducted in ginseng cultivation ecosystems in Northeast China. The t1/2 (half-life) of trifluorocide in ginseng fresh roots, plants, and soil were 8.3–13.1 days, 7.4–10.9 days, and 8.8–10.6 days, respectively. The terminal residues of trifluorocide in ginseng fresh roots were less than 0.01 mg kg−1 after 35 days of trifluorocide application. This study could be beneficial in residue analysis and assist in the scientific application of trifluorocide during ginseng cultivation.
研究领域:
植物保护
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环境科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Can Zhang,Shuo Li,Jing Wu,Tengteng Ping,Ling Ma,Ke Wang,Kaoqi Lian
More and more attention has been paid to undesirable chemical contaminants from food raw materials and ingredients. The study aimed to fabricate novel hydroxyl-functionalized magnetic porous organic polymer Fe 3 O 4 @SiO 2 -NH 2 @Ph-POP and explore its use as magnetic adsorbents for magnetic solid-phase extraction (MSPE) for extracting 31 amide herbicides from fruit wine samples prior to high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Several operational parameters were optimized and the as-prepared magnetic polymer displayed favorable extraction efficiency. The method also showed low limits of detection (0.015–1.412 μg·L -1 ) and limits of quantitation (0.049–4.707 μg·L -1 ). Recoveries for all of the herbicides in four different spiked level samples were between 65.06 % and 101.95 % with intra-day and inter-day relative standard deviations less than 9.89 % and 10.54 %, respectively. The proposed MSPE-HPLC-MS/MS method was successfully applied to simultaneously determine 31 amide herbicides in fruit wine.
研究领域:
分析化学
·
食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Foods
·
2023
·Vol. 12
·期 15
·2875
·
IF 5.2
Yibo Dong,Xiaolong Yao,Wanping Zhang,Xiaomao Wu
3,4-dichloroaniline (3,4-DCA) and 3,5-dichloroaniline (3,5-DCA) are, respectively, the primary metabolites deriving from the breakdown of phenylurea herbicides and dicarboximide fungicides in both soils and plants, whose residues in vegetable products have a heightened concern considering their higher health risks to humans and greater toxicity than the parent compounds in the environment. In this study, a sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous determination of 3,4-DCA and 3,5-DCA residues in chive products based on the optimization of HPLC-MS/MS chromatographic and mass-spectrometric conditions using the standard substances and the modified QuEChERS preparation technique. The preparation efficiency of 3,4-DCA and 3,5-DCA from chive samples showed that acetonitrile was the best extractant. The combination of the purification agent graphite carbon black + primary secondary amine and the eluting agent acetonitrile + toluene (4:1,v/v) had a satisfactory purification effect. The linear correlation coefficients (R2) were more than 0.996 with the six concentration range of 0.001–1.000 mg/L for 3,4-DCA and 3,5-DCA. The limit of detection and limit of quantitation of this method was 0.6 and 2.0 µg/kg for 3,4-DCA, as well as 1.0 and 3.0 µg/kg for 3,5-DCA, respectively. The matrix effect range of 3,4-DCA and 3,5-DCA in chive tissues was from −9.0% to −2.6% and from −4.4% to 2.3%, respectively. The fortified recovery of 3,4-DCA and 3,5-DCA in chive samples at four spiked levels of 0.001–1.000 mg/kg was 75.3–86.0% and 78.2–98.1%, with the relative standard deviation of 2.1–8.5% and 1.4–11.9%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.6, 2.0, and 1.0, 3.03 for 4-DCA and 3,5-DCA, respectively. This study highlights that the analytical method established here can efficiently and sensitively detect residues of 3,4-DCA and 3,5-DCA residues for monitoring chive products. The method was successfully applied to 60 batches of actual vegetable samples from different regions.Keywords:3,4-dichloroaniline;3,5-dichloroaniline;simultaneous determination;UPLC-MS/MS;chive
研究领域:
分析化学
·
食品安全
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF SOLID STATE CHEMISTRY
·
2021
·
IF 3.498
FuKai Li,Min Wang,Jian Zhou,MengRui Yang,TongTong Wang
A novel magnetically and efficiently multifunctional boronic acid (BA) -functionalized core-shell nanohybrid (Fe 3 O 4 @SiO 2 @BA) was prepared for capture and separation of cis -diol-flavonoids. The morphology and physicochemical properties of resultant nanoparticles were systematically characterized via several techniques, and the results confirmed that the target nanohybrids were successfully functionalized and modified. Meanwhile, two flavonoids (quercetin and luteolin) were selected to investigate the selective capture of the Fe 3 O 4 @SiO 2 @BA in procedure of magnetic solid phase extraction (MSPE). The main parameters influencing the adsorption and elution conditions were systematically investigated and optimized. Furthermore, the adsorption kinetic models were adopted to elucidate the adsorption process , indicating that the pseudo-second-order model was suitable to explain the adsorption kinetics. Under the optimum conditions, the MSPE-HPLC-MS/MS approach was established with a wide linear dynamic range and good linearity (R 2 > 0.999), low limits of detection (0.0096–0.033 μg L −1 ) and satisfactory recoveries (91–107.6%). The proposed analytical method was successfully applicated by determining the content of target flavonoids in food samples (apple and onion). Accordingly, the prepared nanohybrid could serve as an efficient, rapid and economical potential adsorbent for extracting cis -diol-flavonoids in complex food samples.
研究领域:
纳米技术
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分析化学
·
食品科学
✓ 已验证
DOI
高影响因子
CURRENT PHARMACEUTICAL BIOTECHNOLOGY
·
2021
·Vol. 22
·期 5
·672-681
·
IF 2.837
Wang Hai-Qiao,Gong Xiao-Mei,Lan Fen,Zhang Yi-Han,Xia Jin-Er,Zhang Hai,Guo Jia-Lin,Liu Min
Background: Timosaponin A-III is one of the most promising active saponins from Anemarrhena asphodeloides Bge. As an oral chemotherapeutic agent, there is an urgent need to clarify its biopharmaceutics and pharmacokinetics to improve its development potential. Objective: This research
explores the bioavailability of timosaponin A-III and clarifies its absorption and metabolism mechanisms by a sensitive and specific HPLC-MS/MS method. Methods: Pharmacokinetics and bioavailability studies of timosaponin A-III were performed in Sprague- Dawley rats by oral (20 mg/kg)
and intravenous administration (2 mg/kg). Control group was given the same volume of normal saline. The absorption of timosaponin A-III was investigated in a rat intestinal perfusion model in situ and a Caco-2 cell transport model in vitro. The metabolic rate of timosaponin A-III was determined
in a rat liver microsome incubation system. Results: After the oral administration, timosaponin A-III reached Cmax of 120.90 ± 24.97 ng/mL at 8 h, and the t1/2 was 9.94 h. The absolute oral bioavailability of timosaponin A-III was 9.18%.
The permeability coefficients of timosaponin A-III in four intestinal segments ranged from 4.98 to 5.42 10-7 cm/s, indicating a difficult absorption. A strikingly high efflux transport of timosaponin A-III was found, PappBA 3.27 ± 0.64 10−6
cm/s, which was abolished by a P-gp inhibitor. Rat liver microsome incubation studies showed that timosaponin A-III could hardly be metabolized, with a t1/2 of over 12 h. In addition, the solubility test showed a low solubility in PBS solution, i.e. 30.58 μg/mL.
Conclusion: Timosaponin A-III exhibited low oral bioavailability by oral and intravenous administration, which was probably caused by its low permeability and solubility. This study may provide a reference for its rational clinical use and further study on the pharmacology or toxicology of
timosaponin A-III.
研究领域:
药理学
·
生物制药学
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中药学
✓ 已验证
DOI
PubMed
高影响因子
MOLECULES
·
2018
·Vol. 23
·期 3
·543
·
IF 3.098
Zhi-Feng Li,Meng-Ying Zhou,Ting Tan,Chen-Cong Zhong,Qi Wang,Shi-Lin Yang,Yu-Lin Feng,Hui Ouyang
Ziyuglycoside I (ZGS1) is a promising drug candidate for the treatment of leucopenia. Currently, information on ZGS1 and its in vivo metabolite ziyuglycoside II (ZGS2) is limited. The objective of this study was to investigate the pharmacokinetics, tissue distribution, and excretion of ziyuglycoside I (ZGS1) and its metabolite ziyuglycoside II (ZGS2) in rats. In our study, a simple and sensitive high-performance liquid chromatography-mass spectrometry (HPLC-MS/MS) method was established for simultaneous determination of ZGS1 and its metabolite for Sprague-Dawley rat pharmacokinetics studies. The method was validated following internationally-approved guidelines. The results presented in this study indicated that subcutaneous administration of ZGS1 prolonged its extension time and increased the area under the curve (AUC0–t) of ZGS2 during 0 to t minutes. In summary, in this study, the pharmacokinetic characteristics of ZGS1 and its metabolite ZGS2 were defined and its tissue distribution, and excretion in rats were described. Our finding may be beneficial for leucopenia drug that focus on ZGS1.Keywords:ziyuglycoside I (ZGS1);ziyuglycoside II (ZGS2);LC-MS/MS;pharmacokinetics;tissue distribution;excretion
研究领域:
药物代谢
·
药理学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）