NUCLEAR MEDICINE AND BIOLOGY
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2026
·
IF 3.1
Lei Xu,Zhenhao Dong,Hong Zhang,Antonio Arleques Gomes,Wagner de Rossi,Jing Wang,Arian Pérez Nario,Qinggang He
A post-column derivatization high-performance liquid chromatography-ultraviolet (HPLC-UV) method was developed to determine Kryptofix 2.2.2 (K2.2.2) in PET tracers. This method utilizes the specific complexation between K2.2.2 and Pb 2+ , forming a stable 1:1 host-guest complex. The complexation produces a bathochromic shift in UV absorption maximum (from 210 nm to 254 nm), enabling sensitive detection. This approach addresses the limitations of poor performance and narrow applicability associated with direct single-method detection of K2.2.2. The chromatographic conditions were optimized (column flow rate: 0.7 mL·min −1 ; derivatization reagent flow rate: 0.7 mL·min −1 ; Pb 2+ concentration: 50 μg·mL −1 ) and the method was validated. The results exhibited excellent linearity (1–100 μg·mL −1 , r 2 > 0.999), high reproducibility (relative standard deviation (RSD) < 5%), and a low detection limit (0.5 μg·mL −1 ). The method successfully quantified K2.2.2 in [ 18 F]FDG, [ 18 F]AV45 and [ 18 F]DPA714, achieving spiked recoveries of 89%–105%. Additionally, the method remained unaffected by interference from common sample components such as sodium chloride and sodium ascorbate. This method provides a novel and efficient quality control tool for the simultaneous analysis of radiochemical purity and K2.2.2 content in diverse PET tracers.
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JOURNAL OF SEPARATION SCIENCE
·
2026
·Vol. 49
·期 5
·e70433
·
IF 3.6
Menghong Xie,Guxi Huang,Hao Wang,Jiazhen Wei,Junliang Lin,Yipeng Huang,Guihua Ruan
Toxic amide herbicide residues pose significant risks to food safety and environmental health. In this study, an ultrasound-assisted dispersive liquid‒liquid extraction method utilizing a hydrophobic menthol-based deep eutectic solvent (DES) was developed for the efficient separation and determination of four amide herbicides in complex matrices, including vegetables, soil, and water. DES composed of decanoic acid (hydrogen bond acceptor) and menthol (hydrogen bond donor) at a molar ratio of 2:3 demonstrated superior extraction performance compared to those using lauric or oleic acid as a hydrogen bond acceptor. The extraction was equilibrated within 2 min under neutral pH conditions. Molecular docking simulations revealed that the N─H groups in the amide moieties served as the primary active sites for hydrogen bonding interactions with the DES. By integrating this green extraction technique with high-performance liquid chromatography, a robust analytical method was established, exhibiting excellent linearity ( R 2 > 0.9991) over a wide range (1–200 ng mL −1 ), with low limits of detection (0.3–0.5 ng mL −1 ) and high precision (intraday RSDs ≤ 3.6%, inter-day RSDs ≤ 8.2%). The method achieved high recoveries (89.8%–116%) across various samples. Greenness assessments using the GAREEprep and Analytical Ecological Scale showed scores of 0.57 and 85, respectively, underscoring the sustainability of the method. This study presents a rapid, sensitive, and sustainable alternative for monitoring amide herbicide residues, contributing to food safety and environmental protection.
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MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Jia-qi Wen,Qing-nan Chen,Hui-xin Ji,Xiao-ting Zhang,Shuang Hu,Yun-e Bai,Jian-ping Gao
A vortex-assisted dispersive liquid-liquid microextraction was proposed based on hydrophobic deep eutectic solvent and high performance liquid chromatography for the quantitative study of five small molecular compounds (tangshenoside I, lobetyolinin, lobetyolin, lobetyol, atractylenolide III) and quality evaluation of Codonopsis Radix. In this experiment, the primary factors impacting the extraction competence process were optimized. Under optimal conditions that were DES (methyltrioctylammonium chloride: glycerol, molar ratio 1:4, 70 μL), pH = 7, vortex time of 90 s, centrifugal time of 2 min, enrichment factors of 6.0, 6.2, 18.9, 58.7, 63.2 for tangshenoside I, lobetyolinin, lobetyolin, lobetyol, atractylenolide III were obtained. The detection limits of the above five components were respectively 9, 6, 2, 0.1, 0.6 µg/L and five analytes had excellent linearities in individual linear ranges ( R 2 > 0.990). Good precision and recovery were 0.5%-8.8% and 92.3%-111.5%. The quantitative results revealed that the proposed approach is quick, simple, feasible, and could accurately detect the contents of five target analytes in 18 batches samples. Finally, five components could be chemical markers to objectively distinguish different specifications of Codonopsis Radix by analysis of variance, further contributing a foundation for quality evaluation and control of Codonopsis Radix.
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Analytical Methods
·
2022
·Vol. 14
·期 47
·4938-4946
·
IF 3.532
Wanliang Liao,Yang Xu,Dingyun Li,Yixing Ye,Yuhan Ning,Weiping Wang,Ai-jun Wang
In this study, a functionalized magnetic covalent organic framework (NiFe2O4@TAPB-TPA) was fabricated with NiFe2O4 nanoparticles as the magnetic core, and 1,3,5-tris(4-aminophenyl)benzene (TAPB) and terephthalaldehyde (TPA) as building blocks by a facile room temperature strategy. Benefitting from the π–π stacking and hydrogen bond interaction, NiFe2O4@TAPB-TPA showed great potential as a magnetic adsorbent for the extraction of tetracyclines (TCs). Under optimal conditions, good linearities (R2 > 0.9990) were obtained between the peak area and TC concentration in the range of 1–500 μg L−1 with limits of detection ranging from 0.09 to 0.26 μg L−1. The intra-day and inter-day relative standard deviations were less than 2.2% and 4.7%, respectively. The established method was successfully applied for the determination of TCs in diverse environmental water samples with satisfactory recoveries in the range of 91.6–102.7%. In addition, NiFe2O4@TAPB-TPA showed good reusability with the recoveries for TCs higher than 73.1% after nine recycles, indicating potential application of NiFe2O4@TAPB-TPA as an ideal adsorbent for the enrichment of TCs.
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ANALYTICA CHIMICA ACTA
·
2022
·
IF 6.911
Xiaochong Song,Qing Luo,Xiaojia Huang
A new strategy based on online hyphenation of magnetism-enhanced in-tube solid phase microextraction (ME-SPME) and HPLC was developed for speciation of organotin compounds (OTCs) in water and seafood samples. Task specific porous polymer embedded magnetic nanoparticles (TPM) was fabricated in capillary and utilized as the microextraction column (MEC) of ME-SPME. The implement of magnetic field during extraction duration obviously improved extraction efficiencies of prepared TPM/MEC towards studied TOCs from 48.0-77.0% to 84.2–99.7%. Under the optimized extraction parameters, sensitive and automatic approach for the quantification of TOCs was developed by online hyphenation of ME-SPME and HPLC with fluorescence detection. The limits of detection for water and seafood samples were in the ranges of 0.0030–1.5 μg/L and 0.71–14 μg/kg, respectively. The established method was employed to measure low contents of studied OTCs in actual samples, and the recoveries at different fortified contents varied from 80.2% to 116% with satisfactory reproducibility (RSDs below 10%). In addition, confirmation experiments were adopted to inspect the accuracy of introduced method.
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MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 2
·1-10
·
IF 5.479
Li Weixia,Chen Ning,Zhu Yan,Shou Dan,Zhi Minyu,Zeng Xiuqiong
A novel nanocomposite consisting of an amorphous seed and a molecularly imprinted covalent organic framework shell was prepared via a heterogeneous nucleation and growth method. By using ibuprofen as the dummy template, a molecularly imprinted covalent organic framework (MICOF) with a large surface area was prepared from 1,3,5-triformylbenzene and 4,4'-diaminobiphenyl. It was placed on the surface of monodisperse amorphous seeds. Owing to strong π-interaction, the MICOF@SiO 2 nanocomposite displays fast binding kinetics, large adsorption capacities and selectivity for nonsteroidal anti-inflammatory drugs (NSAIDs). Following desorption from the MICOF@SiO 2 with methanol containing 1% ammonium hydroxide, the NSAIDs ketoprofen, ibuprofen, diclofenac, indomethacin, flurbiprofen and naproxen were quantified by HPLC with UV detection. Under optimized conditions, the method exhibits good linearity within the range of 0.002–1.0 μg mL-1, low limits of detection (0.38–2.92 μg L-1), and acceptable repeatability. The recoveries of NSAIDs at three spiking levels range from 77 to 112%, and the RSDs are <9.4%. The method was successfully applied to the analysis of NSAIDs in spiked environmental water samples.
A molecular imprinted covalent organic framework nanocomposite (MICOF@SiO 2 ) was prepared by heterogeneous nucleation and growth method. It was explored as a sorbent for the solid phase extraction of nonsteroidal anti-inflammatory drugs before determination by HPLC with UV detection.
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MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Yuxin Zhao,Helong Si,Xinyao Zhao,Hongya Li,Jing Ren,Shuna Li,Quan Wang,Jinlin Zhang
A novel microporous structure monolithic polymer was prepared via free radical polymerization within a stainless steel column (4.6 mm [i.d.] × 50 mm) for separation of lipopeptide antibiotics. The monolithic column was synthesized using allyl- β -cyclodextrin and methyl methacrylate as co-monomers, triallyl isocyanurate and ethylene glycol dimethacrylate as co-crosslinkers, and azobisisobutyronitrile as an initiator. The optimized monolithic columns were evaluated by scanning electron microscopy, a nitrogen absorption-desorption apparatus, and mercury intrusion porosimetry. The homemade monolithic columns not only had a relatively uniform porosity structure, low back pressure, and good permeability, but also show good separation performance. For low molecular weight substances, six aromatic compounds were separated in 6 min and the column efficiency of naphthalene achieved 35, 660 plates m −1 . The enantiomers of ibuprofen and ephedrine, which were used as standard samples, were separated by the homemade monolithic column. The application potential of the monolithic column for the separation of Chinese medicine bioactive substances was illustrated by the ephedrine and pseudoephedrine, which were successfully detected in a crude extract of ephedra. Based on the excellent separation performance of the column for the aforementioned low molecular weight substances, we assumed that there are many forces, such as hydrogen bonds, π - π bonds, and dipole-dipole interactions, that are involved between enantiomers and allyl- β -cyclodextrin. Thus, natural lipopeptide antibiotics in the fermentation broth were used as samples to verify the assumption. Eighteen peaks were precisely separated from the fermentation broth . Among the 18 peaks, 4 lipopeptide antibiotics were identified by mass spectrometry. Methodologic validation was confirmed using two enantiomers of ibuprofen, and all parameters meet the testing requirements.
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FOOD CHEMISTRY
·
2021
·
IF 7.514
Xu Jing,Xin Huang,Huihui Wang,Haoyue Xue,Beiqi Wu,Xiaowen Wang,Liyan Jia
To simultaneously determine the enantiomers of prothioconazole and its chiral metabolite prothioconazole-desthio in water, beer, Baijiu, and vinegar samples by HPLC, a simple, fast, environmentally-friendly popping candy-assisted dispersive liquid–liquid microextraction technique was developed. A green medium-chain fatty acid (decanoic acid) and popping candy could be used as the extractant and solid dispersant respectively to avoid the use of toxic organic solvents. Decanoic acid was collected after extraction by solidification at room temperature. The linear range of this technique was from 27.1 to 1000 µg L −1 . The limits of detection and quantification were within the ranges of 8.1–11.2 μg L -1 and 27.1–37.3 μg L -1 , respectively. The extraction recovery was 80.8% to 102.5% with the relative standard deviation ranged from 1.1 to 7.1%. This technique has been successfully applied to enantioselectively determine the residues of prothioconazole and prothioconazole-desthio in water, beer, Baijiu, and vinegar samples.
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MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Fukai Li,Min Wang,Jian Zhou,MengRui Yang,TongTong Wang
A novel cyclodextrin-derivatized hybrid magnetic nanocomposite, denoted as Fe 3 O 4 @SiO 2 @CD, was fabricated and employed as the adsorbent of magnetic solid-phase extraction (MSPE) for preconcentration of elven fluoroquinolones (FQs) from water samples. The prepared nanoparticles exhibited excellent magnetic responsiveness (56.7 emu g −1 ), uniform size distribution (about 300 nm), good thermal and chemical stability, excellent reusability and superior chemical affinities to the target FQs via hydrogen bond, host–guest inclusion complexation and π–π interactions. Under the optimized conditions, the MSPE was coupled with HPLC-MS/MS to sensitively quantify trance levels of FQs in environmental water. The developed method revealed satisfactory precision with RSDs lower than 4%, good linearity (R 2 ≥ 0.9981), low limits of detection (0.0014–0.023 µg L −1 ) and satisfactory recoveries (93.2–105%). Furthermore, the proposed approach was validated by analyzing the Certified Reference Material of GBW 10152 and GBW 10153 chicken meat powder. These results demonstrated that the Fe 3 O 4 @SiO 2 @CD nanoparticles are a promising magnetic adsorbent for FQs, and the established MSPE-HPLC-MS/MS approach is suitable for simultaneous analysis of trace levels of FQs in actual samples.
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Journal of Pharmaceutical Analysis
·
2020
·
IF 2.673
Yuan Hong,Xiaoyan Liao,Zilin Chen
The fruits of leguminous plants Cercis Chinensis Bunge are still overlooked although they have been reported to be antioxidative because of the limited information on the phytochemicals of C. chinensis fruits. A simple, rapid and sensitive HPLC-MS/MS method was developed for the identification and quantitation of the major bioactive components in C. chinensis fruits. Eighteen polyphenols were identified, which are first reported in C. chinensis fruits. Moreover, ten components were simultaneously quantified. The validated quantitative method was proved to be sensitive, reproducible and accurate. Then, it was applied to analyze batches of C. chinensis fruits from different phytomorph and areas. The principal components analysis (PCA) realized visualization and reduction of data set dimension while the hierarchical cluster analysis (HCA) indicated that the content of phenolic acids or all ten components might be used to differentiate C. chinensis fruits of different phytomorph.
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JOURNAL OF APPLIED MICROBIOLOGY
·
2020
·Vol. 129
·期 5
·1410-1418
·
IF 3.066
Li Z.,Liu Y.,Li Y.,Lin F.,Wu L.
AimsRed yeast rice (RYR), produced by inoculating Monascus strains to steamed rice, contains many kinds of physiologically bioactive compounds, among which monacolin K can be used as an antihypercholesterolaemic agent. However, RYR can be polluted by the mycotoxin citrinin, which has nephrotoxic and hepatotoxic activities. To avoid the risk of citrinin contamination in Monascus fermented products, it is important to screen for Monascus strains that produce no or low citrinin.Methods and ResultsFive autochthonous Monascus strains with high‐yield monacolin K and undetectable citrinin were obtained using high‐performance liquid chromatography (HPLC). All five strains were identified as Monascus ruber based on Genealogical Concordance Phylogenetic Species Recognition criteria. Polymerase chain reaction revealed that citrinin polyketide synthase (pksCT) gene was found in these strains, but transcriptional regulator (ctnA) was not found.ConclusionsFive strains are potential strains for producing high‐quality RYR. The distribution of the pksCT gene was not restricted to Monascus purpureus and Monascus sanguineus, and M. ruber strains were diverse in pksCT and ctnA genes.Significance and Impact of the StudyThe integration of citrinin HPLC analysis and pksCT and ctnA genes amplification could provide a complementary approach in valuable Monascus strains screening.
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Chinese Medicine
·
2020
·Vol. 15
·期 1
·1-19
·
IF 2.96
Chang Shanquan,Wang Mei,Tian Yushan,Qi Jin,Qiu Zhixia
Background Zengye decoction (ZYD) has been widely used in the treatment of type 2 diabetes mellitus (T2DM). Exploring the fate of various components of ZYD in vivo is of considerable significance for pharmacological research and molecular mechanism elaboration. However, the systematic analysis on the metabolic behavior of chemical components of ZYD in T2DM rats has not been reported. Methods To screen and characterize the complex chemical compositions of ZYD, and metabolism fate in plasma, urine, bile, and feces of T2DM rats, the model of T2DM rats was prepared. A rapid procedure using high-performance liquid chromatography coupled with electrospray ionization quadrupole time of flight tandem mass spectrometry (HPLC-ESI-Q-TOF–MS/MS) was established. Data were acquired and analyzed by Agilent MassHunter Workstation Qualitative Analysis software version B.07.00 and PCDL manager B.07.00. Results A total of 80 compounds were identified or tentatively characterized in ZYD, 31 more than previously detected. Besides, 36 prototype components and 49 metabolites of ZYD were found and characterized in T2DM rats, and the proposed fragmentation pathways and possible metabolic behaviors of the main types of compounds were described. Conclusions This study developed the understanding of the composition of ZYD as well as the cleavage rules and metabolic pathways of the prototype compounds. Besides, this study provided abundant data for further research and for study of the metabolism of traditional Chinese medicine prescriptions.
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