Analytical Methods
·
2021
·Vol. 13
·期 29
·3264-3273
·
IF 2.896
Jia Xu,Cao Li,Xiao Li,Yuxiu Xiao
A novel extraction technique i.e. hydrophobic magnetic nanoparticle (MNP)-assisted in situ supramolecular solvent (SUPRAS) microextraction was proposed, and it was applied for the analysis of sulfonamides (SAs) and fluoroquinolones (FQs) in aqueous samples, coupled with high performance liquid chromatography-UV detection (HPLC-UV). In this extraction method, hexafluoroisopropanol-mediated salt-free catanionic surfactant based SUPRAS in situ microextraction was initially carried out; then, the SUPRAS was quickly adsorbed by the hydrophobic magnetic nanoparticles and gathered by an external magnetic field. This can greatly shorten the separation time and overcome the dependence on centrifugation, and also perform a secondary extraction of free analytes (not extracted by SUPRAS) from water samples. The magnetic separation ability of different hydrophobic MNPs was evaluated by adsorbing supramolecular aggregates from the water sample. The effective parameters affecting the extraction efficiency of the analytes were investigated and optimized using the one variable at a time method. About 3 min was required to realize the extraction of analytes with an enrichment factor (EF) of 12–53 for SAs and 79–118 for FQs. Compared with the centrifugation-assisted SUPRAS microextraction, the hydrophobic MNP-assisted SUPRAS microextraction obtained much better extraction and preconcentration efficiency. The proposed novel extraction method with HPLC-UV provided LODs of 0.21–0.76 ng mL−1 for SAs and 0.10–0.18 ng mL−1 for FQs. Good linearity was obtained with correlation coefficients ranging from 0.9962 to 0.9999. The intra- and inter-day recoveries of the target antibiotics were in the range of 92.0–111.3% with RSD% below 10.4%. The method was successfully applied to determine SAs and FQs in real water samples, such as lake water, river water, reservoir water, and wastewater.
研究领域:
分析化学
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环境科学
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纳米技术
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高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Xin Wang,Xiyue Li,Qian Tian,Chengyan Zhang,Xiaoyun Lei,Zuoping Zhao
HP-γ-CD-grafted zwitterionic copolymer enables PT-μSPE of FQs. • Complementary γ-CD and MPC sites provide recognition and matrix tolerance. • DFT calculations support complementary hydrogen-bonding and electrostatic interactions. • PT-μSPE-HPLC-UV enables FQ determination in milk and honey. The trace determination of fluoroquinolone antibiotics (FQs) in animal-derived foods requires effective sample pretreatment to minimize matrix interference and improve analytical sensitivity. Herein, a pipette-tip micro solid-phase extraction method coupled with high-performance liquid chromatography and ultraviolet detection (PT-μSPE-HPLC-UV) was developed for the determination of FQs in food samples. A porous zwitterionic cyclodextrin-based copolymer was synthesized as the PT-μSPE sorbent. The copolymer integrates hydroxypropyl-γ-cyclodextrin (HP-γ-CD) cavities with zwitterionic phosphorylcholine groups, combining host-guest recognition, hydrogen bonding, electrostatic interactions, and antifouling hydration to improve analyte enrichment and matrix tolerance. Density functional theory (DFT) calculations suggested complementary recognition in the hybrid system, which exhibited generally shorter hydrogen-bond distances than those calculated for the zwitterionic monomer-only models and electrostatic potential extrema of greater magnitude than those of γ-CD alone. Under the optimized conditions, the method exhibited good linearity over the range of 1.0 to 500 μg L⁻¹, limits of detection of 0.07 and 0.24 μg L⁻¹, and limits of quantification of 0.23 and 0.72 μg L⁻¹ for lomefloxacin and gatifloxacin, respectively. Recoveries in spiked milk and honey ranged from 74.8% to 110.3%, and norfloxacin and enrofloxacin were also effectively enriched. The proposed miniaturized method provides a simple, economical, and practical approach for FQs enrichment and screening in complex food matrices. Download: Download high-res image (206KB) Download: Download full-size image
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2026
·
IF 5.3
Mengmeng Feng,Yongkang Luo,Yanfei Jiang,Chunyue Zhao
α-Ketoglutarate (AKG), ergothioneine (EGT), ascorbic acid (VC), and pyrroloquinoline quinone (PQQ) are increasingly co-formulated to combat age-related mitochondrial dysfunction and oxidative stress, driving an urgent need for reliable quality control. However, existing analytical approaches remain fragmented, targeting only one or two compounds, relying on time-consuming derivatization, or employing costly mass spectrometry, and critically failing to address chemical incompatibilities among analytes. This study presents the first validated HPLC-UV method for simultaneous quantification of all four bioactives. A segmented extraction strategy was developed to reconcile their physicochemical conflicts: VC, AKG, and EGT were extracted with 0.1% metaphosphoric acid, while acid-labile PQQ was separately extracted with neutral phosphate buffer. Chromatographic separation was achieved on an AQ-C18 column with a gradient of 50 mM Na₂HPO₄ and acetonitrile. The method demonstrated excellent linearity (R² > 0.99), high sensitivity, good precision (RSD < 2%), and satisfactory accuracy (recoveries: 97.2–103.6%). The Mosaic-WAC score of 82.6 further validates the proposed method. Analysis of commercial products indicated that only VC exhibited degradation, with more pronounced losses in liquid matrices, attributable to its inherent oxidizability. This underscores the need for comprehensive multi-component quality control. The proposed method provides a practical platform for routine analysis and regulatory evaluation of complex nutraceutical products.
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Systems Microbiology and Biomanufacturing
·
2025
·
IF 2.9
Shi Yu,Li Huifan,Lu Yuqi,Chen Ming,Yang Hua,Fu Dongmei
A simple and robust reversed-phase high performance liquid chromatography procedure was developed with only an aqueous H 3 PO 4 solution (pH 2.1) as the mobile phase for the simultaneous determination of nine organic acids (oxalic, formic, malic, lactic, acetic, citric, succinic, fumaric, and gallic acids) in beer based on a polar-copolymerized 3-chloropropyl C18 column. The proposed method was validated according to linearity, limits of detection, accuracy, precision, repeatability, and reproducibility. Quantifications of the nine organic acids in 12 commercial Chinese beer samples from five different brands were conducted only after degassing and filtration of the samples. In all beer samples, the most abundant organic acid was succinic acid; its concentration was in the range of 907.99–3557.22 mg/L. This was followed by malic acid (170.39–936.78 mg/L). Principal component analysis was used to compare the different brand of beers according to organic acid concentration, and results may provide a reference for the evaluation of beer quality and taste.
研究领域:
分析化学
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食品科学
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色谱技术
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高影响因子
MICROCHIMICA ACTA
·
2025
·Vol. 192
·期 5
·1-12
·
IF 5.3
Li Weixia,Lei Jiacheng,He Tiancheng,Gan Yaping,Zhu Yan
A novel Zr-based metal–organic framework (MOF) functionalized with graphene oxide-coated allylmethacrylate-divinylbenzene microspheres (AMA/DVB@GO), termed AMA/DVB@GO@UiO-66-NH 2 was designed. The composite exhibits great adsorption capacity and selectivity for bisphenols (BPs), driven by synergistic interactions, including hydrophobic, π-π, and hydrogen bonding. We optimized conditions to establish an efficient dispersive micro-solid phase extraction procedure coupled with high-performance liquid chromatography (d-μSPE-HPLC) for extracting BPs from milk samples, using the AMA/DVB@GO@UiO-66-NH 2 composite. The method achieved recoveries ranging from 84.0 to 106.6%, with relative standard deviations below 6.9% and detection limits between 0.17 and 0.67 μg/L. This study introduced a novel, hydrophilic, and stable AMA/DVB@GO@UiO-66-NH 2 composite, offering a promising material for the selective enrichment and detection of BPs in food analysis. Graphical
研究领域:
食品科学
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分析化学
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PubMed
高影响因子
Current Analytical Chemistry
·
2024
·Vol. 21
·期 2
·124-133
·
IF 1.7
Zhengming Qian,Zhuobin He,Dongyin Lian,Qi Huang,Guoying Tan,Juying Xie
BackgroundFlavonoid is a type of active constituent in herbs and always used as the quality control markers of herbal medicines. Owing to the extensive diversity of flavonoids, numerous reference compounds are necessitated for the analysis of flavonoids, and some are usually very expensive, which engenders challenges in the analysis of flavonoids in herbal medicines. Consequently, the development of a simple, rapid, and reference compounds saving method is important for the determination of flavonoids in herbal medicines.ObjectiveIn order to develop a high-performance liquid chromatography (HPLC) method for the determination of 5 flavonoids (mangiferin, hesperidin, baicalin, buddleoside, and rutin) in five herbal medicines (Anemarrhenae rhizome, Sophorae flos, Citri reticulatae pericarpium, Scutellariae radix, and Chrysanthemi indici flos) with rutin.MethodsFive herbal medicine samples were prepared according to the Chinese Pharmacopoeia which includes ultrasound and reflux methods. The separation of the sample was performed on a PoroShell 120 EC-C18 (4.6 mm×100 mm, 2.7 μm) by gradient elution with 0.1% formic acid and acetonitrile at a flow rate of 1.0 mL/min. The wavelengths were set as follows: Anemarrhenae rhizome (363 nm), Sophorae flos (256 nm), Citri reticulatae pericarpium (236 nm), Scutellariae radix (263 nm), Chrysanthemi indici flos (354 nm).ResultsThe method validation showed that the established HPLC method was accurate and stable for quantitative analysis of flavonoids in five herbal medicines. The comparative analysis revealed that the determination results of the current HPLC method and Chinese Pharmacopoeia method are consistent, exhibiting less than 1% relative error. Remarkably, the developed HPLC method needs one cheapest reference compound (rutin) and costs 8 min for sample HPLC analysis.ConclusionThe developed HPLC method for quantitative analysis of five flavonoids in five herbal medicines is simple, rapid, and reference compound saving, which provides a good alternative method for quality control of flavonoids in herbal medicines.
研究领域:
药学
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分析化学
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高影响因子
MOLECULES
·
2022
·Vol. 27
·期 7
·2088
·
IF 4.927
Xue-Li Liu,Yong-Hui Wang,Shu-Yue Ren,Shuang Li,Yu Wang,Dian-Peng Han,Kang Qin,Yuan Peng,Tie Han,Zhi-Xian Gao,Jian-Zhong Cui,Huan-Ying Zhou
The efficient capture of multi-pollutant residues in food is vital for food safety monitoring. In this study, in-situ-fabricated magnetic MIL-53(Al) metal organic frameworks (MOFs), with good magnetic responsiveness, were synthesized and applied for the magnetic solid-phase extraction (MSPE) of chloramphenicol, bisphenol A, estradiol, and diethylstilbestrol. Terephthalic acid (H2BDC) organic ligands were pre-coupled on the surface of amino-Fe3O4composites (H2BDC@Fe3O4). Fe3O4@MIL-53(Al) MOF was fabricated by in-situ hydrothermal polymerization of H2BDC, Al (NO3)3, and H2BDC@Fe3O4. This approach highly increased the stability of the material. The magnetic Fe3O4@MIL-53(Al) MOF-based MSPE was combined with high-performance liquid chromatography-photo diode array detection, to establish a novel sensitive method for analyzing multi-pollutant residues in milk. This method showed good linear correlations, in the range of 0.05–5.00 μg/mL, with good reproducibility. The limit of detection was 0.004–0.108 μg/mL. The presented method was verified using a milk sample, spiked with four pollutants, which enabled high-throughput detection and the accuracies of 88.17–107.58% confirmed its applicability, in real sample analysis.Keywords:magnetic metal organic framework (MMOFs);magnetic solid-phase extraction (MSPE);multi-pollutants;high-performance liquid chromatography (HPLC)
研究领域:
食品安全
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分析化学
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
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2018
·
IF 3.716
Sijie Zheng,Man He,Beibei Chen,Bin Hu
A melamine-based porous organic polymer (mPMF) was synthesized as solid phase extraction (SPE) adsorbent for inline SPE-high performance liquid chromatography (HPLC)-ultraviolet detector (UV) analysis of five phytohormones. Melamine contributed to the rich π-electron and N-containing triazine structure for mPMF, which could form π-π interaction and intermolecular hydrogen bond with COOH containing phytohormones. The synthesized mPMF adsorbent shows extremely high extraction efficiency for five target analytes (>80%) including salicylic acid, indole-3-acetic acid, abscisic acid, 2,4-dichlorophenoxyacetic acid and 1-naphthalene acetic acid. The factors affecting extraction of the target phytohormones were investigated and the optimized experimental conditions were established. The linear range was 0.2–100 μg/L with the limits of detection in the range of 0.06–0.11 μg/L for five target phytohormones. The developed method of mPMF-inline-SPE-HPLC-UV was applied for the analysis of trace target phytohormones in tomato and grape juice samples, and the recovery in the range of 83.1–116% and 87.2–121% was obtained for the spiked tomato and grape juice, respectively. This method has the advantages of high sensitivity and good reproducibility, and it has good application potential for the analysis of phytohormones in fruit samples. Moreover, inline analysis avoided the problems of sample pollution and sample loss, and provided a sample throughput of 5/h.
研究领域:
分析化学
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植物科学
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食品科学
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高影响因子
Journal of Zhejiang University-SCIENCE B
·
2013
·Vol. 14
·期 7
·604-614
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IF 1.108
Wang Shu-fang,Leng Jing,Xu Yi-min,Feng Mei-ling
Xiongdankaiming tablet (XDKMT), a well-known compound in traditional Chinese medicine, is widely used for the treatment of acute iridocyclitis and primary open-angle glaucoma. In this paper, accurate and reliable methods were developed for the identification of 20 constituents using high-performance liquid chromatography with photodiode array and electron spray ionization-mass spectrometry (HPLC-PDA/ESI-MS n ), and determination of nine of the constituents (chlorogenic acid, gentiopicroside, isochlorogenic acid B, diosmetin-7- O -β- d -glucopyranoside, apigenin, diosmetin, tauroursodeoxycholic acid, acacetin, and taurochenodeoxycholic acid) was developed using HPLC with ultraviolet absorption detector and evaporative light scattering detector (HPLC-UV/ELSD) for the first time. The best results were obtained on a Zorbax SB-C18 column with gradient elution using water (0.1% formic acid) (A) and methanol (0.1% formic acid) (B) at a flow rate of 0.7 ml/min. Tauroursodeoxycholic acid and taurochenodeoxycholic acid, owing to their low UV absorption, were detected by ELSD. The other seven compounds were analyzed by HPLC-UV with variable wavelengths. The calibration curves of all nine constituents showed good linear regression ( R
2 >0.9996) within the linearity ranges. The limits of detection and quantification were in the ranges of 0.0460–9.90 μg/ml and 0.115–24.8 μg/ml, respectively. The accuracy, in terms of recovery, varied from 95.3% to 104.9% with relative standard deviations (RSDs) less than 4.4%. Precision (with the intra- and inter-day variations less than 4.4%) was also suitable for its intended use. The developed method was successfully applied for the analysis of major components in XDKMT, which provides an appropriate method for the quality control of XDKMT.
研究领域:
中药学
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分析化学
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PubMed
高影响因子
NUCLEAR MEDICINE AND BIOLOGY
·
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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高影响因子
MICROCHIMICA ACTA
·
2021
·Vol. 188
·期 2
·1-9
·
IF 5.833
Senosy Ibrahim Abdelhai,Zhang Xin-Zhong,Lu Zhi-Heng,Guan Xiao-Yu,Yang Zhong-Hua,Li Jian-Hong,Guo Hao-Ming,Abdelrahman Talat Mahmoud,Mmby Mohamed,Gbiliy Asmaa
Fe 3 O 4 @MIL-100 (Fe)/PEI are used for the first time as an adsorbent material for the extraction of pesticide residues (epoxiconazole, flusilazole, tebuconazole, and triadimefon) from food matrices. The adsorbent proposed (Fe 3 O 4 @MIL-100(Fe)/PEI) was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), thermogravimetric (TG) analysis, and vibrating sample magnetometer (VSM) techniques to evaluate the properties of the sorbent. Then, the Fe 3 O 4 @MIL-100 (Fe)/PEI was employed for the quantification of the four triazole fungicides in fruits and vegetables (apple, orange, tomato, cabbage, and cucumber) using HPLC-UV for separation and detection. During the extraction process, the main parameters such as amount of adsorbent, extraction time, pH value, ionic strength, eluting solvent, and eluting volume were optimized. Under the optimum conditions, good linearity of this method was observed for all analytes, with correlation coefficients ( R 2 ) ≥ 0.9908. The limits of detection (LODs) ranged from 0.021–3.04 μg kg −1 . The extraction recoveries of the four triazole fungicides varied from 73.9 to 109.4% with relative standard deviations (RSD) in the range 0.5 to 6.2%. Compared with other MOFs, the modification of Fe 3 O 4 @MIL-100 (Fe) with PEI shows high efficient adsorption due to the combined benefits of MIL-100 (Fe) and PEI. The material is easily synthesized, has good stability, and is of low cost.
Graphical abstract
研究领域:
分析化学
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食品安全
·
环境科学
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高影响因子
TALANTA
·
2021
·
IF 6.057
Xin-Qiao He,Yuan-Yuan Cui,Xiao-Hui Lin,Cheng-Xiong Yang
Development of novel functionalized adsorbents for efficient magnetic solid phase extraction (MSPE) is essential for promoting their versatile applications in sample pretreatment. Herein, we report the fabrication of a new polyethyleneimine-600 decorated magnetic microporous organic network nanosphere (Fe 3 O 4 @MON-PEI 600 ) for effective MSPE of trace non-steroidal anti-inflammatory drugs (NSAIDs) from different water samples. The core-shelled Fe 3 O 4 @MON-PEI 600 integrates the synergistic effects of Fe 3 O 4 , MON and PEI 600 , providing facile and effective extraction to NSAIDs via multiple hydrogen bonding , π-π and hydrophobic interactions. The inner MON shell employs π-π and hydrophobic interaction sites and the outer PEI-600 coat acts as the hydrogen bonding doner/receptor, which affords good extraction performance for NSAIDs. Under optimal conditions, the Fe 3 O 4 @MON-PEI 600 -MSPE-HPLC-UV method gives wide linear range (0.14–400 μg L −1 ), low limits of detection (0.042–0.149 μg L −1 ), good precisions (intra-day and inter-day RSDs < 4.5%, n = 6), and large enrichment factors (97.0–98.2). Extraction mechanisms and selectivity of Fe 3 O 4 @MON-PEI 600 are evaluated in detail. Moreover, Fe 3 O 4 @MON-PEI 600 is successfully applied to enrich the trace NSAIDs in different water samples with the concentrations of 0.7 and 0.8 μg L −1 for 1-naphthylacetic acid, 0.5 and 0.1 μg L −1 for naproxen as well as 0.7 μg L −1 for ibuprofen , respectively. The developed method not only affords a novel and efficient magnetic adsorbent for NSAIDs in aqueous media at trace level, but also provides a new strategy for the rational design and synthesis of multiple functionalized MON composites in sample pretreatment.
研究领域:
分析化学
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环境科学
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材料科学
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PubMed
高影响因子
危险品化学品经营许可证（带存储）