ANALYTICAL LETTERS
·
2025
·
IF 1.8
Yi Zhang,Jiali Lu,Jiaxiong Zhao,Genrong Li,Shuai Li
This study presents an efficient and highly sensitive method for detecting Rhodamine B and 6 G in complex food matrices. A dual microextraction approach combining electromembrane extraction (EME) and magnetic solid-phase extraction (MSPE) was applied, followed by analysis using high-performance liquid chromatography with fluorescence detection (HPLC-FLD). Critical parameters—such as donor and acceptor phase pH, applied voltage, membrane solvent, extraction time, sorbent dosage, adsorption duration, and elution conditions—were systematically optimized to ensure reliable and reproducible performance. The method showed excellent linearity (1.0–200 ng/mL; R2 = 0.9987 for Rhodamine B and 0.9983 for Rhodamine 6 G), with detection limits of 0.9 ng/mL and 1.2 ng/mL, respectively. Recoveries ranged from 92.1% to 101.9% with relative standard deviations (RSDs) below 5%. Application to real food samples—including spicy strips, candies, and chili oil-based bean snacks—confirmed the method’s accuracy and strong matrix tolerance. Compared to conventional microextraction-chromatographic techniques, this method offers notable advantages in speed, sensitivity, and broad applicability. It is a powerful tool for rapid screening and regulatory monitoring of illicit synthetic dyes in food.
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高影响因子
CHROMATOGRAPHIA
·
2026
·
IF 1.3
Yang Weiqi,Li Xiaofei,Wang Wenhao,Huang Qi,Fan Hui,Qian Zhengming
Bistorta vivipara L. achenes ( B. vivipara achenes), rich in phenolic acids and flavonoids, are a valuable food and medicinal resource. However, a detailed analysis of its individual components and their mechanisms remains unexplored. This study introduces solid-phase extraction (SPE) for selectively isolating and purifying total phenolic acids and flavonoids from B. vivipara achenes. The antioxidant potential of the extracts was evaluated using ABTS (2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid)), DPPH (2,2-diphenyl-1-picrylhydrazyl), and FRAP (ferric ion reducing antioxidant potential) assays. Results showed significant antioxidant activity in the total phenolic acid extract (125.1 ± 0.7 mg GAE/g dry weight [DW]) and total flavonoid extract (1491.1 ± 19.9 mg RE/g DW). Using online FRAP–high-performance liquid chromatography (FRAP–HPLC), seven antioxidant components were identified in the phenolic acid fraction and thirteen in the flavonoid fraction. Notably, protocatechuic acid, cryptochlorogenic acid, isochlorogenic acid A, isochlorogenic acid B, isochlorogenic acid C, shaftoside, isoshaftoside, isoorientin, taxifolin, and vitexin are reported for the first time as antioxidant constituents in B. vivipara achenes. These findings highlight B. vivipara achenes as a promising source of natural antioxidants and functional food ingredients. The SPE–FRAP–HPLC method enables comprehensive analysis by selectively enriching active compounds and enhancing sensitivity and accuracy compared with crude extracts. Furthermore, the application of online FRAP–HPLC facilitates real-time monitoring of the antioxidant activity of individual compounds during chromatographic separation, providing a detailed antioxidant activity profile of phenolic compounds in B. vivipara achenes. Graphical
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高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2020
·Vol. 43
·期 19
·3775-3784
·
IF 2.878
Shuping Guan,Hao Wu,Liu Yang,Zhuliang Wang,Jianmin Wu
A magnetic covalent organic framework material was synthesized with a core-shell structure using a simple solvothermal method. It was prepared with Fe 3 O 4 as the magnetic core, covalent organic framework as the shell, which synthesized from 1,3,5-triformylphloroglucinol and p -phenylenediamine by Schiff base reaction. Transmission electron microscopy, Fourier transform infrared spectroscopy, powder X-ray diffraction, vibrating sample magnetometry, and nitrogen adsorption-desorption were used to characterize magnetic adsorbent. It has showed a large specific surface area (505.6 m 2 /g), which can provide many adsorption sites. Moreover, the saturation magnetization value was 48.4 emu/g enough to be separated by external magnet. Six kinds of fluoroquinolones (enoxacin, fleroxacin, ofloxacin, norfloxacin, pefloxacin, and lomefloxacin) were extracted by magnetic solid phase extraction with the magnetic adsorbent. High-performance liquid chromatography detects the entire adsorption and desorption process to further evaluate the optimal extraction and desorption conditions. Under the optimal chromatographic conditions, this method showed a low detection limit (0.05 to 0.20 μg/L), good linearity in the range of 0.5 to 200 μg/L, and the enrichment factor reaches 115.5-127.3. The spiked recovery of the fluoroquinolones in milk sample ranged from 90.4 to 101.2%.
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PubMed
高影响因子
ANALYTICAL LETTERS
·
2022
·
IF 2.267
Hui Cao,Zixin Chen,Yanan Kong,Ziqi Wei,Tai Ye,Min Yuan,Jinsong Yu,Xiuxiu Wu,Liling Hao,Fengqin Yin,Fei Xu
Rapid dispersive liquid-liquid microextraction (DLLME) based on the solidification of a switchable hydrophilicity solvent (SHS) was established for the preconcentration of pyrethroid pesticides from grain prior to determination using high‐performance liquid chromatography (HPLC) with photodiode array (PDA). Lauric acid was selected to be the switchable hydrophilicity solvent due to its conversion between hydrophobic and hydrophilic forms and solidification at low temperature, thereby avoiding a time-consuming centrifugation step. The results show that the optimal conditions for pyrethroid pesticides included 30 mmol/L lauric acid, hydrochloric acid as the hydrogen donor, a 1:1.8 stoichiometric ratio of sodium laurate and hydrochloric acid, an extraction temperature of 50 °C, an extraction time of 8 min, and a solidification time of 3 min. Under the optimal conditions, this approach provided a high enrichment factor (308.4 to 330.2), a short pretreatment period of less than 15 min, and sensitive detection limits from 5 to 20 ng/g suitable for the analysis of food. The method was employed for the determination of pyrethroid pesticides in grain. The recoveries were 84.3% to 115.7%, and the relative standard deviation was less than 9.9%.
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高影响因子
MOLECULES
·
2018
·Vol. 24
·期 1
·64
·
IF 3.098
Peiying Shi,Chunlei Yang,Ya Su,Liying Huang,Xinhua Lin,Hong Yao
This study has developed a reliable and precise high performance liquid chromatography-tandem mass spectrometry method for the simultaneous determination of five phenolic acids and four flavonoid glycosides in rat plasma after a single intravenous administration of Kudiezi injection (KI). Chromatographic separation was carried out on an Ultimate®XB-C18column (4.6 × 100 mm, 3.5 μm) using a gradient elution program with a mobile phase consisting of water containing 0.5% acetic acid and acetonitrile at a flow rate of 0.6 mL/min. Detection was performed on a triple-quadrupole tandem mass spectrometry using multiple reaction monitoring in negative electrospray ionization mode. The calibration curves of all analytes showed good linearity (R2> 0.990). The results of selectivity, intra-day and inter-day precisions, extraction recoveries, matrix effects and stability were satisfactory. Pharmacokinetic parameters showed that luteolin-7-O-β-d-gentiobioside, luteolin-7-O-β-d-glucuronide, luteolin-7-O-β-d-glucoside and apigenin-7-O-β-d-glucuronide were eliminated quickly (0.07 h
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PubMed
高影响因子
MOLECULES
·
2018
·Vol. 23
·期 4
·714
·
IF 3.098
Weijuan Du,Lisha Jin,Liping Li,Wei Wang,Su Zeng,Huidi Jiang,Hui Zhou
The tuber ofCorydalis yanhusuois a famous traditional Chinese medicine and found to have potent pharmacological effects, such as antinociceptive, antitumor, antibacterial, anti-inflammatory, and anti-depressive activities. Although there are several methods to be developed for the analysis and detection of the bioactive ingredients’ alkaloids, so far, only few prominent alkaloids could be quantified, and in vitro and in vivo changes of comprehensive alkaloids after oral administration are still little known. In this study, we first developed a simple and sensitive high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) method to quantify the comprehensive alkaloids of extracts ofC. yanhusuoin mouse plasma, using nitidine chloride as an internal standard. As results, at least fourteen alkaloids, including an aporphine (oxoglaucine), a protopine (protopine), five tertiary alkaloids (corydaline, tetrahydroberberine, tetrahydropalmatine, tetrahydrocolumbamine, and tetrahydrocoptisine) and seven quaternary alkaloids (columbamine, palmatine, berberine, epiberberine, coptisine, jatrorrhizine, and dehydrocorydaline) could be well quantified simultaneously in mouse plasma. The lower limits of quantification were greater than, or equal to, 0.67 ng/mL, and the average matrix effects ranged from 96.4% to 114.3%. The mean extraction recoveries of quality control samples were over 71.40%, and the precision and accuracy were within the acceptable limits. All the analytes were shown to be stable under different storage conditions. Then the established method was successfully applied to investigate the pharmacokinetics of these alkaloids after oral administration of the extract ofCorydalis yanhusuoin mice. To the best of our knowledge, this is the first document to report the comprehensive and simultaneous analyses of alkaloids ofC. yanhusuoin mouse plasma. It was efficient and useful for comprehensive pharmacokinetic and metabolomic analyses of these complex alkaloids after drug administration.Keywords:alkaloids;Corydalis yanhusuoextract;pharmacokinetics;HPLC-ESI-MS/MS;oxoglaucine
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高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 12
·2528-2540
·
IF 2.557
Jinmao You,Kun Dou,Cuihua Song,Guoliang Li,Zhiwei Sun,Shijuan Zhang,Guang Chen,Xianen Zhao,Na Hu,Wu Zhou
A rapid, sensitive, and selective precolumn derivatization method for the simultaneous determination of eight thiophenols using 3-(2-bromoacetamido)- N -(9-ethyl-9 H )-carbazol as a labeling reagent by high-performance liquid chromatography with fluorescence detection has been developed. The labeling reagent reacted with thiophenols at 50°C for 50 min in aqueous acetonitrile in the presence of borate buffer (0.10 mol/L, pH 11.2) to give high yields of thiophenol derivatives. The derivatives were identified by online postcolumn mass spectrometry. The collision-induced dissociation spectra for thiophenol derivatives gave the corresponding specific fragment ions at m/z 251.3, 223.3, 210.9, 195.8, and 181.9. At the same time, derivatives exhibited intense fluorescence with an excitation maximum at λ ex = 276 nm and an emission maximum at λ em = 385 nm. Excellent linear responses were observed for all analytes over the range of 0.033–6.66 μmol/L with correlation coefficients of more than 0.9997. Detection limits were in the range of 0.94–5.77 μg/L with relative standard deviations of less than 4.54%. The feasibility of derivatization allowed the development of a rapid and highly sensitive method for the quantitative analysis of trace levels of thiophenols from some rubber products. The average recoveries ( n = 3) were in the range of 87.21–101.12%.
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高影响因子
ANALYTICAL LETTERS
·
2024
·
IF 1.6
Jingjing Gu,Chunyang Chen,Tingting Liu,Yanyan Li,Xuedong Wang
Here is reported effervescent reaction-enhanced switchable hydrophilic-hydrophobic solvent-based salting-out microextraction (ERSSM) with high-performance liquid chromatography with photodiode array detection (HPLC-PDA) for the preconcentration, extraction, and trace-level determination of polybrominated diphenyl ethers (PBDEs) in milk and water. The important variables were rigorously optimized to be 150 µL of hexanoic acid as the extraction solvent, 400 µL of Na2CO3 as the alkaline source, 350 µL of H2SO4 solution as the acid source, and NaCl as the salting-out agent. The optimized conditions provided a linear range from 0.2 to 50 µg L−1 with limits of detection and quantitation from 0.026 to 0.085 µg L−1 and 0.087 to 0.28 µg L−1 for six PBDEs. The intra-day and inter-day precision values were from 2.48% to 6.75%, and the fortified recoveries for PBDEs were between 78.06% and 103.07% in water and milk samples. The developed procedure avoids the use of a traditional organic disperser and mechanical mixing allowing the determination of PBDEs outdoors by synchronous extraction method and high efficiency for the analytes. These advantages suggest a high potential for the routine monitoring of PBDEs in liquid food and environmental samples.
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高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2020
·Vol. 412
·期 30
·8339-8350
·
IF 3.637
Gao Yue,Tan Jiangkun,Lu Jiao,Sun Zhiwei,Li Zan,Ji Zhongyin,Zhang Shijuan,You Jinmao
In this study, a novel fluorescent labeling reagent 2-(9-acridone)-ethyl chloroformate (AEC-Cl) was designed, synthesized and applied for the determination of free amino acids by high-performance liquid chromatography with a fluorescence detector (HPLC-FLD). The free amino acids were rapidly and efficiently labeled by AEC-Cl in the presence of basic catalyst (pH 9.0) within 5 min at room temperature (25 °C). The derivatives exhibited excellent stability and fluorescence properties, with maximum excitation and emission wavelengths at 268 nm and 438 nm, respectively. Derivatives of 22 kinds of natural amino acids were completely separated by gradient elution on a Hypersil ODS C18 column. Under the optimal conditions, the calibration curves exhibited excellent linear responses, with correlation coefficients of R 2 > 0.9994. The detection and quantification limits were in the range of 0.61–2.67 μg kg −1 and 2.07–8.35 μg kg −1 , respectively. Therefore, AEC-Cl was successfully applied for the detection of trace levels of free amino acids in honey samples.
A novel fluorescent labeling reagent was applied for the determination of free amino acids in honey by high-performance liquid chromatography with a fluorescence detector.
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高影响因子
CHIRALITY
·
2021
·Vol. 33
·期 12
·938-950
·
IF 2.437
Shirong Cao,Chunting Xie,Qianyun Ma,Shaoping Wang,Jiayu Zhang,Zhaokun Wang
In the present study, an accurate, rapid, and simple chiral HPLC-UV method with amylose tris(3-chloro-5-methylphenylcarbamate) as stationary phase was developed and applied for enantiomeric determination of six nonsteroidal anti-inflammatory drugs (NSAIDs) in the commercial pharmaceutical formulations, including ( R , S )-ibuprofen, S-ibuprofen, ( R , S )-ketoprofen, S-ketoprofen, S-naproxen, and ( R , S )-loxoprofen sodium. Experiments on the influence of mobile phase composition, proportion of organic modifier, percentage of acid additives, and column temperature on enantioseparation were conducted to obtain the best separation condition. It was indicated that one mobile phase simply composed of acetonitrile-water (0.1% formic acid, v/v) at the proportion of 50:50 (v/v) with a flow rate of 0.6 ml/min at 22°C could simultaneously provide the excellent enantiomeric resolutions for all selected NSAIDs, which made the enantioseparation process more applicable and operable. The newly developed method was then applied for determination of NSAID enantiomers in pharmaceutical formulations containing racemic mixtures or single stereoisomers. Calibration curve of each enantiomer at the concentration of 5.0–100 ug/ml showed good linearity with the correlation coefficient above 0.9996. Satisfactory recovery (96.54–101.54%), good intra-day precision (RSD 0.52–1.46%), and inter-day precision (RSD 0.13–1.09%) were also obtained. The newly developed method was then applied for determination of NSAID enantiomers in pharmaceutical formulations containing racemic mixtures or single stereoisomers. Quantitative results of the commercial capsules and tablets demonstrated that the difference between the declared and measured values did not exceed 1.52%.
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高影响因子
ANALYTICAL LETTERS
·
2022
·
IF 2.267
Lanying Xu,Yingying Huang,Bingshan Zhao,Limin Ren,Tao Long
β-Cyclodextrin modified magnetic microspheres were synthesized and used as an effective adsorbent for the solid-phase extraction of three phenols from water samples. Scanning electron microscopy and Fourier transform infrared spectrometry were used to characterize the adsorbents. The major parameters affecting the extraction and desorption efficiencies, such as adsorbent dosage, extraction time, pH, ionic strength, and eluent type were systematically optimized. Under these conditions, three phenols in water samples were extracted and determined by high performance liquid chromatography (HPLC) with diode array detection (DAD). Limits of detection (LODs) of 0.04–0.34 ng mL−1 and limits of quantification (LOQs) from 0.13 to 1.14 ng mL−1 were achieved with good repeatability (relative standard deviation <7.5%). The developed method was applied for the determination of 2,4-dichlorophenol, 2,4-dinitrophenol and bisphenol A in spiked Yangtze River water, and the recoveries were from 81.0% to 94.9%. The results demonstrated that the combination of magnetic solid-phase extraction (MSPE) with HPLC-DAD is suitable for the determination of trace phenolics in environmental water.
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高影响因子
MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 4
·1029-1036
·
IF 4.58
Zhou Qingxiang,Lei Man,Li Jing,Liu Yongli,Zhao Kuifu,Zhao Danchen
Metal organic frameworks of type MOF-5 exhibit good adsorption capacity for many organic compounds. The authors have used nanoscale silica-coated zerovalent iron and MOF-5 to prepare, by co-precipitation, a novel magnetic nanomaterial of type Fe@MOF-5. Its morphology and structure were characterized by transmission electron microscopy and X-ray diffraction. The nanomaterial is shown to be well suited for magnetic solid phase extraction for five kinds of N- and S-containing polycyclic aromatic hydrocarbons prior to quantitation by HPLC. The limits of detection are in the 25 to 33 ng⋅L −1 concentration range. Four real water samples were used to validate the method, and the recoveries of spiked samples with concentrations of 5 and 10 ppb were found to be in the range between 92.6 and 97.3% ( n = 3). The Fe@MOF-5 sorbent obviously has excellent adsorption capability for such compounds, can be fairly easily synthesized, displays sensitivity, simplicity, ease of operation, and can be prepared at low costs. In our perception, it has a large potential in terms of monitoring such environmental pollutants.
A metal organic framework of type Fe@MOF-5 is found to exhibit good adsorption capacity for N- and S-containing polycyclic aromatic hydrocarbons. A sensitive magnetic solid phase extraction method with Fe@MOF-5 was developed for the determination of N- and S-containing polycyclic aromatic hydrocarbons from the water samples.
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高影响因子
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