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FOOD CHEMISTRY · 2021 · IF 7.514

A highly sensitive and selective method for the determination of ceftiofur sodium in milk and animal-origin food based on molecularly imprinted solid-phase extraction coupled with HPLC-UV

Guohao Cheng,Juan Zhao,Xiaoyue Wang,Can Yang,Shiying Li,Tong Lu,Xiang Li,Xuefeng Wang,Guifen Zhu

The effective analysis of cephalosporin antibiotics in food animals has attracted considerable attention. Herein, a high-performance liquid chromatograph equipped with a UV method based on molecularly imprinted-solid phase extraction (MISPE-HPLC-UV) was developed for preconcentration, cleanup and determination of ceftiofur sodium (CTFS) in food samples. In this method, an eco-friendly molecularly imprinted polymer (MIP) was synthesized and employed as an adsorbent, which exhibited excellent selectivity towards CTFS in water, and adsorption equilibrium could be reached within 1 h. Under the optimized conditions, good linearity was obtained for CTFS in the range of 0.005–1.0 mg L −1 with a lower LOD of 0.0015 mg L −1 , and the average recoveries were higher than 91.9% (RSD less than 8.5%) at three spiked levels in milk, chicken, pork and beef samples. After 20 cycles, the recovery of the MISPE cartridge for CTFS was still higher than 95%, which proved that the MISPE-HPLC-UV method was highly sensitive and selective for the analysis of CTFS in food samples.

CAS / MDL: 443-48-1
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RSC Advances · 2019 ·Vol. 9 ·期 12 ·6717-6723 · IF 3.049

Development of a HPLC-FL method to determine benzaldehyde after derivatization with N-acetylhydrazine acridone and its application for determination of semicarbazide-sensitive amine oxidase activity in human serum

Xiuli Dong,Jiayuan Tang,Yan Ren,Xiangming Chen

A novel fluorescence labeling reagent N-acetylhydrazine acridone (AHAD) was designed and synthesized. A highly sensitive high performance liquid chromatography (HPLC) method coupled with fluorescence detection to determine benzaldehyde after derivatization with AHAD was developed. Optimum derivatization was obtained at 40 °C for 30 min with trichloroacetic acid as catalyst. Benzaldehyde derivative was separated on a reversed-phase SB-C18 column in conjunction with a gradient elution and detected by fluorescence detection at excitation and emission wavelengths of 371 nm and 421 nm. The established method exhibited excellent linearity over the injected amount of benzaldehyde of 0.003 to 5 nmol mL−1. The method was successfully applied to the determination of serum semicarbazide-sensitive amine oxidase (SSAO) activity in humans. SSAO is a significant biomarker because serum SSAO activity is elevated in patients with Alzheimer's disease, vascular disorders, heart disease and diabetes mellitus. It was demonstrated that the SSAO activity of the hyperglycemic group (60 ± 4 nmol mL−1 h−1) was significantly higher than that of normal blood sugar group (44 ± 4 nmol mL−1 h−1) with P < 0.05.

CAS / MDL: 100-46-9 100-52-7
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MICROCHIMICA ACTA · 2020 ·Vol. 187 ·期 1 ·1-9 · IF 6.232

A nanocomposite consisting of etched multiwalled carbon nanotubes, amino-modified metal-organic framework UiO-66 and polyaniline for preconcentration of polycyclic aromatic hydrocarbons prior to their determination by HPLC

Chen Jianxiong,Zhang Birong,Dang Xueping,Zheng Dongyun,Ai Youhong,Chen Huaixia

A polyaniline composite doped with etched multi-walled carbon nanotubes and UiO-66-NH 2 was prepared by electropolymerization. It was used as a sorbent to extract the polycyclic aromatic hydrocarbons (PAHs) phenanthrene, fluoranthene and pyrene. Its surface morphology, crystal structure and capability of adsorbing PAHs were characterized by scanning electron microscopy, X-ray photoelectron spectrometry, Fourier transform infrared spectrometry and zeta potentiometry. The π stacking and anion-π interactions are shown to play dominant roles in the sorption mechanism. Coupled with high performance liquid chromatography, the composite-modified fiber was applied to detect PAHs in lake water samples by direct immersion extraction. The method excels by (a) wide linear range (0.05–20 ng mL −1 ), (b) low limits of detection (10 pg mL −1 ), (c) satisfactory recovery from spiked samples (84.7–113.8%), and (d) good reproducibility (relative standard deviations of <6.5%). The method is superior in terms of costs and reproducibility compared to some pretreatment methods with mass spectrometric detection. Schematic representation for interaction between PANI-etched MWCNT/UiO-66-NH 2 and polycyclic aromatic hydrocarbons (phenanthrene, fluoranthene, pyrene).

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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2014 · IF 2.694

Simultaneous determination of five free and total flavonoids in rat plasma by ultra HPLC–MS/MS and its application to a comparative pharmacokinetic study in normal and hyperlipidemic rats

Xiaofan Wang,Xu Zhao,Liqiang Gu,Chunxiao Lv,Bosai He,Zhenzhen Liu,Pengyi Hou,Kaishun Bi,Xiaohui Chen

A simple and rapid ultra-high performance liquid chromatography–tandem mass spectrometry (uHPLC–MS/MS) method has been developed for the simultaneous determination of five free flavonoids (amentoflavone, isorhamnetin, naringenin, kaempferol and quercetin) and their total (free and conjugated) forms, and to compare the pharmacokinetics of these active ingredients in normal and hyperlipidemic rats. The free and total forms of these flavonoids were extracted by liquid–liquid extraction with ethyl acetate. The conjugated flavonoids were deconjugated by the enzyme β-Glucuronidase and Sulfatase. Chromatographic separation was accomplished on a ZORBAX Eclipse XDB-C 8 USP L7 column using gradient elution. Detection was performed on a 4000Q uHPLC–MS/MS system from AB Sciex using negative ion mode in the multiple reaction monitoring (MRM) mode. The lower limits of quantification were 2.0–5.0   ng/mL for all the analytes. Intra-day and inter-day precision were less than 15% and accuracy ranged from −9.3% to 11.0%, and the mean extraction recoveries of analytes and internal standard (IS) from rat plasma were all more than 81.7%. The validated method was successfully applied to a comparative pharmacokinetic study of five free and total analytes in rat plasma. The results indicated that the absorption of five total flavonoids in hyperlipidemia group were significantly higher than those in normal group with similar concentration–time curves.

CAS / MDL: 56-04-2
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Science China-Chemistry · 2013 ·Vol. 56 ·期 11 ·1641-1650 · IF 1.327

HPLC-DAD data coupled with second-order calibration method applied to food analysis: Simultaneous determination of six benzoylurea insecticides in various fruit samples by selecting time region of chromatogram

Qing XiangDong,Wu HaiLong,Nie ChongChong,Li Yong,Yan XiuFang,Zhang XiHua,Yin XiaoLi,Yu RuQin

This work presents a novel application of second-order calibration based on self-weighted alternating trilinear decomposition (SWATLD) algorithm for analyzing the HPLC-DAD data. The proposed method makes it possible to simultaneously determine teflubenzuron, hexaflumuron, flufenoxuron, chlorfluazuron, diflubenzuron and benzoylurea in different fruit samples, i.e. pear, apple and banana, in the selected time region of chromatogram. The concentration, elution time and spectral information of these benzoylurea insecticides are selectively extracted from complex matrices even in the presence of unknown interferences. The root-mean-square error of prediction (RMSEP) and figures of merit, including sensitivity (SEN), selectivity (SEL) and limit of detection (LOD) are employed to access the performance of the method. The LODs obtained for these insecticides are within the range 0.017–0.26 ppm in pears, 0.039–0.33 ppm in apples, 0.041–0.44 ppm in bananas, respectively. Such a chemometrics-based protocol holds great potential to be extended as a promising alternative for more practical applications in food safety and quality monitoring.

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FOOD CHEMISTRY · 2025 · IF 9.8

Development of a semi-automated one-step purification method for determination of 63 pesticides in fish samples by HPLC-MS/MS using natural loofah sponge as a novel adsorbent

Yupeng Wen,Wendi Huo,Xinyuan Zhang,Yingchun Mu,Huan Liu,Chaoying Zhang,Lu Qiao,Jincheng Li

In this study, we developed a miniaturized semi-automatic purification method based on pressure-filtration purification for sensitive HPLC-MS/MS monitoring of pesticides in aquatic products. For the first time, loofah sponge was demonstrated and utilized as a novel green, low-cost, and effective one-step purification adsorbent for fish sample. The developed method consisted of two main steps: first, target analytes were extracted from fish samples using an acetonitrile-based QuEChERS extraction method. Subsequently, the extract was automatically purified through a pressure-filtration purification column in a centrifuge, followed by HPLC-MS/MS analysis. Under optimized experimental conditions, the method exhibited excellent linearity, with a range of 1.0 to 50.0 μg/kg and a correlation coefficient > 0.99. The detection and quantification limits were 0.5 and 1–2 μg/kg, respectively. Recoveries at spiked levels of 2.0, 5.0 and 30.0 μg/kg ranged from 69.95 to 104.88 %, with intra-day RSDs ranging from 0.58 to 15.01 % and inter-day RSDs ranging from 0.72 % to 14.32 %.

CAS / MDL: 631-61-8 64-19-7 64-18-6
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FOOD CHEMISTRY · 2024 · IF 8.5

Comparative study on the enzymatic degradation of phenolic esters: The HPLC-UV quantification of tyrosol and gallic acid liberated from tyrosol acyl esters and alkyl gallates by hydrolytic enzymes

Xinmiao Wang,Qian Wang,Dong Cai,Jinghan Yu,Xuan Chen,Xu Guo,Peiyong Tong,Xiaoyang Liu,Fawen Yin,Dayong Zhou

HPLC-UV analysis was used to evaluate the enzymatic degradation characteristics of tyrosol acyl esters (TYr-Es) and alkyl gallates (A-GAs). Among various hydrolytic enzymes, TYr-Es can be hydrolyzed by pancrelipase, while A-GAs cannot be hydrolyzed by pancrelipase. Interestingly, carboxylesterase-1b (CES-1b), carboxylesterase-1c (CES-1c) and carboxylesterase-2 (CES-2) are able to hydrolyze TYr-Es and A-GAs, and thus to liberate tyrosol (TYr) and gallic acid (GA). By contrast, the degrees of hydrolysis (DHs) of TYr-Es and A-GAs by CES-1b and CES-1c were significantly higher than those by CES-2. Meanwhile, the DHs of TYr-Es were much higher than those of A-GAs. Especially, the DHs firstly increased and then decreased with the increasing alkyl chain length. Besides, DHs positively correlated with the unsaturation degree at the same chain length. Through regulating carbon length, unsaturation degree and the ester bond structure, controlled-release of phenolic compounds and fatty acids (or fatty alcohols) from phenolic esters will be easily achieved.

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CHEMICAL ENGINEERING JOURNAL · 2025 · IF 13.2

An ultrastable tetraazacalix[2]arene[2]triazine functionalized MXene for highly selective and sensitive determination of p-Phenylenediamines and their quinone derivatives in environmental water via HPLC-MS/MS

Yichan Huo,Xiong Wang,Yang Yi,Zhirong Yang,Wenchang Wang,Huaijie Yao,Pingping Liu,Wenfen Zhang,Shusheng Zhang

p -Phenylenediamine antioxidants (PPDs) and their quinone derivatives (PPDQs) have emerged as concerning environmental contaminants due to their widespread presence and biological toxicity. Herein, a novel tetraazacalix[2]arene[2]triazine functionalized 2D transition metal carbide (TCT@MXene) with electron-rich and electron-deficient sites, porous structures, abundant adsorption sites was first synthesized and characterized. Combining the advantages of extraordinary adsorption capacities and rates towards PPDs and PPDQs, a dispersive solid-phase extraction coupled with high-performance liquid chromatography-mass spectrometry (HPLC-MS/MS) strategy was developed for highly sensitive and selective determination of PPDs and PPDQs in environmental water. The method featured acceptable linearity (R 2  ≥ 0.999), high sensitivity (LOD ranged from 0.10 to 2.96 ng L −1 ), and qualified precision (RSD ≤ 5.90 %). Compared with published works, the LODs of the developed technique were improved 3.8–250 times. Furthermore, its exceptional thermal and chemical stability allows for at least 10 reuse cycles under varying pH conditions. The adsorption mechanism revealed that the complementary charge distribution and robust conjugated system of TCT@MXene enabled the simultaneous and efficient co-adsorption of both PPDs and PPDQs. Besides, the established method was successfully applied to the analysis of trace targets in Yellow River basin in Henan Province. All these results proved the promising application of the developed method for organic pollutants analysis in water samples.

CAS / MDL: 101-54-2 101-72-4
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THERAPEUTIC DRUG MONITORING · 2025 · IF 2.4

A Sensitive Ultrafiltration Plus RP-HPLC-FLD Method to Quantify Total and Free Perampanel Concentrations in the Plasma of Patients With Epilepsy: A Fully Validated Assay With Clinical Application

Dong Zhonghua,Wang Peng,Cui Xueyan,Liu Jinjuan,Shi Haiyan,Yang Yilei,Xu Jingya,Yi Qiaoyan

Background: Perampanel (PER), a novel antiepileptic drug, exhibits high protein binding. Given the drug's susceptibility to various factors, including drug interactions, and the considerable variability in blood concentrations among individuals, solely measuring the total plasma concentration of PER may not provide comprehensive insights. This study aimed to establish an HPLC-FLD method to quantify both total and free PER in clinical samples. Methods: Analysis of total PER involved a straightforward sample preparation process involving plasma protein precipitation. Plasma samples were ultrafiltered to isolate the free portion of PER. Chromatographic separation was achieved on an InertSustain C18 column at a 1-mL/min flow rate using a gradient of acetonitrile and aqueous sodium acetate buffer at pH 4.4. Results: Calibration curves for total and free PER in plasma exhibited excellent linearity over the concentration ranges of 10–3000 and 0.5–100 ng/mL, respectively. The method was applied to analyze blood samples from patients with epilepsy quantitatively; the total concentration of perampanel in the plasma of the patients was in the range of 90.45–563.39 ng/mL, whereas the free concentration was in the range of 1.82–15.29 ng/mL. The plasma protein binding ratio of perampanel was normally between 97.09% and 99.29% and decreased in cases of hypoproteinemia. Conclusions: The method was rigorously validated for selectivity, accuracy, precision, and stability in accordance with established FDA and EMA guidelines. The developed method enables the rapid and accurate quantification of both total and free PER concentrations in the plasma of patients with epilepsy, offering technical support for its subsequent clinical application.

CAS / MDL: 127-09-3
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MICROCHIMICA ACTA · 2019 ·Vol. 186 ·期 5 ·1-9 · IF 5.479

Simultaneous HPLC-MS determination of 8-hydroxy-2′-deoxyguanosine, 3-hydroxyphenanthrene and 1-hydroxypyrene after online in-tube solid phase microextraction using a graphene oxide/poly(3,4-ethylenedioxythiophene)/polypyrrole composite

Chen Dan,Xu Hui

The exploration of monohydroxy polycyclic aromatic hydrocarbons and 8-hydroxy-2′-deoxyguanosine (8-OHdG) produced by oxidative stress and DNA damage is a powerful and non-invasive tool to study the health risk of exposure to polycyclic aromatic hydrocarbons (PAHs). A nanocomposite prepared from graphene oxide, poly(3,4-ethylenedioxythiophene) and polypyrrole was electrodeposited on the internal surface of a stainless-steel tube for online in-tube solid phase microextraction (IT-SPME) of 8-OHdG, 3-hydroxyphenanthrene and 1-hydroxypyrene from urine. The coating possesses excellent chemical and mechanical stability, high extraction efficiency, good resistance to matrix interference, and a long lifespan. An online IT-SPME-high performance liquid chromatography-mass spectrometry method was developed for the determination of these three metabolite biomarkers in human urine. Figures of merit include (a) enrichment factors of 30–48; (b) low limits of detection (4–41 pg·mL −1 at S/ N  = 3); (c) wide linear ranges (0.05–50 ng·mL −1 ); (d) good recoveries from spiked samples (71.6–109.5%); and (e) acceptable repeatability (2.3–14.6%). The method offers the advantages of low cost, simplicity, sensitivity, rapidity and automation. Schematic illustration of online in-tube solid phase microextraction using graphene oxide/poly(3,4-ethylenedioxythiophene)/polypyrrole composites as adsorbent in a stainless-steel (SS) tube for the enrichment and simultaneous determination of 8-hydroxy-2′-deoxyguanosine, 3-hydroxyphenanthrene and 1-hydroxypyrene prior to HPLC-MS analysis.

研究领域: 分析化学 · 环境健康 · 毒理学
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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment · 2020 · IF 2.34

Development and establishment of a QuEChERS-based extraction method for determining tembotrione and its metabolite AE 1417268 in corn, corn oil and certain animal-origin foods by HPLC-MS/MS

Kai Cui,Xiaohu Wu,Lusheng Zhu,Ying Zhang,Gaochen Dai,Junli Cao,Jun Xu,Fengshou Dong,Xingang Liu,Yongquan Zheng

In this study, we established a rapid and sensitive HPLC-MS/MS method for quantitative determination of tembotrione and its metabolite AE 1417268 (M5) in corn, corn oil, beef, pork, chicken, and eggs. Both analytes eluted from a C18 column within 6 min. The electrospray ionisation–positive mode was used for tembotrione, whereas the negative mode was used for M5. Acetonitrile was the extractant for all samples, and the addition of 2 g NaCl to each homogenised sample facilitated the extraction of the analytes into acetonitrile. The extracted analytes were further purified by the addition of 50 mg of C18 sorbent (25 mg GCB was also added to corn samples) for subsequent HPLC-MS/MS analysis. Satisfactory calibration-curve linearities (R2 ≥ 0.997) were obtained for the two analytes at concentrations of 1–500 μg/L. Mean recoveries in different matrices ranged from 73.7% to 110.4%, whereas intra-day and inter-day relative standard deviations were <15% for all concentrations of spiked analytes. The limit of quantification was 2 μg/kg for each analyte in all matrices. In food samples obtained from markets, residual tembotrione and M5 were all below the limits of quantification. These results confirm that the method is suitable for the routine monitoring of residual tembotrione and M5 in a variety of food matrices.

研究领域: 食品科学 · 分析化学
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MOLECULES · 2023 ·Vol. 28 ·期 14 ·5309 · IF 4.6

A New HPLC-UV Method Using Hydrolyzation with Sodium Hydroxide for Quantitation of Trans-p-Hydroxycinnamic Acid and Total Trans-p-Hydroxycinnamic Acid Esters in the Leaves of Ligustrum robustum

Shi-Hui Lu,Xiao-Na Liang,Xiao-Jin Nong,Ran Chen,Xiu-Xia Li

Trans-p-hydroxycinnamic acid and its esters in the leaves ofLigustrum robustummight be a new resource to prevent diabetes and its complications. In the present study, a new HPLC-UV method using hydrolyzation with sodium hydroxide for quantitation oftrans-p-hydroxycinnamic acid and totaltrans-p-hydroxycinnamic acid esters in the leaves ofL. robustumwas developed, since it was difficult and troublesome to analyze no less than 34trans-p-hydroxycinnamic acid esters by usual HPLC. The extract ofL. robustumwas hydrolyzed with sodium hydroxide at 80 °C for 2 h, and then, hydrochloride was added. HPLC analysis was performed in reverse phase mode using a C-18 column, eluting with methanol-0.1% acetic acid aqueous solution (40:60,v/v) in isocratic mode at a flow rate of 1.0 mL·min−1and detecting at 310 nm. The linear range fortrans-p-hydroxycinnamic acid was 11.0–352.0 μg·mL−1(r2= 1.000). The limit of detection and limit of quantification were 2.00 and 6.07 μg·mL−1, respectively. The relative standard deviations of intra-day and inter-day variabilities fortrans-p-hydroxycinnamic acid were less than 2%. The percentage recovery oftrans-p-hydroxycinnamic acid was 103.3% ± 1.1%. It is the first HPLC method using hydrolyzation for quantification of many carboxylic esters. Finally, the method was used successfully to determinetrans-p-hydroxycinnamic acid and totaltrans-p-hydroxycinnamic acid esters in various extracts of the leaves ofL. robustum. The 60–70% ethanol extracts ofL. robustumshowed the highest contents of freetrans-p-hydroxycinnamic acid (3.96–3.99 mg·g−1), and the 50–80% ethanol extracts ofL. robustumdisplayed the highest contents of totaltrans-p-hydroxycinnamic acid esters (202.6–210.6 mg·g−1). The method can be applied also to the quality control of the products ofL. robustum.Keywords:trans-p-hydroxycinnamic acid;esters;Ligustrum robustum;HPLC-UV;hydrolyzation;sodium hydroxide;quantification

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