JOURNAL OF CHROMATOGRAPHY A
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2018
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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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DOI
PubMed
高影响因子
SEPARATION AND PURIFICATION TECHNOLOGY
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2022
·
IF 9.136
Lu Liu,Sinan Lu,Haiyan Liu,Ligai Bai
Stemonae Radix shows multiple pharmacological effects, mainly due to the alkaloid of tuberostemonine contained in it. An online SPE-HPLC method was fabricated by combining the solid-phase extraction (SPE) cartridge with a C18 analytical column through high-performance liquid chromatography (HPLC) system, which was used for the quantitative determination of tuberostemonine from Stemonae Radix extract and plasma. The SPE cartridge shows excellent matrix removal ability and specific selectivity for the tuberostemonine. The methodology validation confirms its good accuracy with the spiked recovery of 100.6%∼101.7%, a good repeatability with the relative standard deviations of 0.3%∼0.7% ( t R ) and 5.8%∼7.7% ( A ). Furthermore, the proposed monolithic SPE cartridge was used for the preparative separation and purification of tuberostemonine from Stemonae Radix, which was carried out on a semi-preparative HPLC instrument, with a high yield of 1.08 mg g −1 obtained. These results show that the present monolithic cartridge is an outstanding SPE adsorbent for the extraction, separation, enrichment and purification of tuberostemonine from Stemonae Radix, which can be extended to the analysis of similar alkaloids from complex samples.
研究领域:
生药学
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分析化学
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药学
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DOI
高影响因子
TALANTA
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2016
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IF 4.035
Xinpeng Dai,Xiuna Jia,Pan Zhao,Ting Wang,Jian Wang,Peiting Huang,Lu He,Xiaohong Hou
As a novel kind of materials, metal-organic frameworks (MOFs) have great potential for the preconcentration of trace analytes. In our work, MIL-101(Cr) was prepared and applied as a solid phase extraction (SPE) sorbent for the pretreatment of sulfadiazine (SDA), sulfamethazine (SMZ), sulfachloropyridazine (SCP) and sulfamethoxazole (SMX) in different environmental water samples coupling with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) detection. Experimental parameters, such as SPE materials, pH of water sample, volume of sample, flow rate , and type and volume of elution solvent, were properly optimized. Under the optimum conditions, good sensitivity levels were achieved with the detection limits of 0.03–0.08 μg/L and the quantitation limits of 0.11–0.27 μg/L. The linear ranges were from 0.2–40 or 0.5–100 μg/L ( r 2 >0.996) for the analytes, and the relative recoveries were in the range from 83.5% to 107.3% with the relative standard deviations (RSD) between 0.2% and 8.0% ( n =6). In addition, computational simulation was primarily used to predict the adsorption of MIL-101(Cr) toward sulphonamides (SAs), and also demonstrated the molecular interactions and free binding energies with the molecular modeling method. The results revealed that the combination of experimental and computational study not only accurately recognized the adsorption of MIL-101(Cr) on SAs, but also provided a new strategy on the trace contaminant analysis.
研究领域:
环境科学
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分析化学
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DOI
高影响因子
FOOD CHEMISTRY
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2026
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IF 10.4
Jiajun Chen,Nan Zhu,Feixuan Wang
A simultaneous detection of MDA/4-HHE/4-HNE method is developed by UHPLC-QqQ-MS/MS. • Optimized derivatization and purification reduced interference from lipid impurities. • This validated method showed high sensitivity/precision with low LOD/LOQ. • Micrograms per kilogram level sensitivity capably monitors lipid peroxidation in oily food. A novel and sensitive method using ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS) was developed for the simultaneous determination of three lipid oxidation markers: malondialdehyde (MDA), 4-hydroxy-2-hexenal (4-HHE), and 4-hydroxy-2-nonenal (4-HNE) in edible oils and nuts. Optimization of 2,4-dinitrophenylhydrazine (DNPH) derivatization and solid-phase extraction (SPE), combined with isotope compensation to ensure high analytical performance: linearity ( R ≥ 0.9990), precision (RSD ≤ 18.75%), accuracy (SD ≤ 19.24%), recovery (80.34–119.78%). Limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.25 to 0.50 μg/kg and 0.50–2.50 μg/kg, respectively. This validated method was further applied to monitor lipid peroxidation levels, revealed that thermal processing significantly increases MDA/4-HHE/4-HNE contents, which reached 7.80 mg/kg from 26.50 μg/kg in oils and 0.98 mg/kg from 8.27 μg/kg in nuts. Notably, the accumulation of MDA and 4-HHE in edible oils was approximately tenfold higher than in nuts. A novel and sensitive method using UHPLC-QqQ-MS/MS was developed for the simultaneous determination of three lipid oxidation markers: MDA, 4-HHE and 4-HNE in edible oils and nuts. Optimization of DNPH derivatization and SPE, combined with isotope compensation to ensure high analytical performance. Download: Download high-res image (119KB) Download: Download full-size image
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2016
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IF 2.687
R. Xu,H.T. Gao,F. Zhu,W.X. Cao,Y.H.M. Yan,X. Zhou,Q. Xu,W.L. Ji
This research was mainly focused on the effects of food emulsifier on the bioavailability of six priority controlling phthalate acid esters (PAEs) for the further accurate assessment of their toxic effects, using the corresponding phthalate acid monoesters (PAMEs) in rats urine as biomarkers. Glycerin monostearate was chosen as typical food emulsifier. A method was established to determine PAMEs in urine from rats either in experimental group (integrated gavaged with glycerin monostearate and PAEs) or in control group (gavaged with PAEs only), by using solid-phase extraction (SPE) coupled with ultra performance liquid chromatography tandem mass spectrometry (SPE–UPLC–MS/MS). Extraction recoveries were more than 75% for all the PAMEs; the calibration curve was linear in the range of 1.0–1000.0 ng/mL with R 2 > 0.995; the limits of detection (LOD) were 0.30 ng/mL–0.50 ng/mL. In addition, by analysing quality control (QC) urine samples in 3 days, it showed that the method was precise and accurate, for the intra-day and inter-day RSD within 16%, and the accuracy more than 82%. Internal exposure amount of all PAEs in experimental group was significantly higher than that in control group with p values of less than 0.05 except for butyl benzyl phthalates (BBP) ( P = 0.07). The bioavailability of all PAEs ranged from 5.03% to 109.35% with the presence of food emulsifiers glycerin monostearate, observably higher than that without glycerin monostearate (1.12% to 54.39%). It indicated that food emulsifiers increased the bioavailability of PAEs and may lead to potential food safety risk, which should bring awareness and be further studied.
研究领域:
毒理学
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分析化学
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食品安全
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DOI
PubMed
高影响因子
ANALYTICAL LETTERS
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2022
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IF 2.267
Xu-Feng Wang,Qiang Wang,Jin-Lan Yang,Dong-Hao Zhao
An amino-modified multiwalled carbon nanotube (MWCNT) solid-phase extraction-based hydrophilic interaction liquid chromatography–tandem mass spectrometry (HILIC–MS/MS) method was developed for simultaneous determination of 13 paralytic shellfish toxins (PSTs) in bivalve mollusks. Shellfish samples were extracted with 1% acetic acid followed by cleanup using optimized MWCNT-NH2 based solid-phase extraction. Absorbed PSTs were eluted with 2 mL 1% acetic acid–acetonitrile (70/30, v/v). The separation was performed on a Waters BEH Amide column within 7.5 min utilizing 0.1% formic acid–acetonitrile and 2 mM ammonium acetate containing 0.1% formic acid as the mobile phase. The analytes were quantified by matrix-matched external standard curves with correlation coefficients® exceeding 0.997 acquired in multiple reaction-monitoring mode. The limits of detection and quantitation in shellfish samples were from 2.76 to 9.8 μg/kg and 9.11 to 39.3 μg/kg, respectively. Recoveries at three spiked levels ranged from 71.4% to 97.8% with relative standard deviations less than 12.6%. The developed method was satisfactorily applied to the analysis of shellfish.
研究领域:
分析化学
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食品安全
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DOI
高影响因子
INSTRUMENTATION SCIENCE & TECHNOLOGY
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2022
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IF 1.509
Shan Wang,Yamei Han,Jiangwei Chen,Ligai Bai,Hongyuan Yan,Haiyan Liu
A metal organic framework (MOF)-based monolithic column was prepared by in situ polymerization using modified MIL-101-NH2 and glycidyl methacrylate (GMA) as monomers. The monolithic column was used as a solid phase extraction (SPE) adsorbent for on-line enrichment and preliminary purification of diosmetin in traditional Chinese medicine. After being characterized by scanning electron microscopy (SEM) and nitrogen adsorption-desorption, the advantages of the monolithic column with MIL-101-NH2 added were reflected in the pore structure and specific surface area. The monolithic column for SPE had a linear relationship from 0.13 µg/mL to 5.0 × 102 µg/mL. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.04 µg/mL and 0.13 µg/mL, respectively. The recovery was from 96% to 104%, and the intra-day and inter-day relative standard deviations (RSDs) were below 1.1%. This method was suitable for the determination of diosmetin in complex samples.
研究领域:
分析化学
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药学
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材料科学
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产品关联
DOI
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
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2026
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IF 4.1
Zhou Xinyue,Duan Sufei,Lou Yuye,Deng Yue,Feng Shuang,Liu Jiale,Zhang Jiarui,Xi Yalin,Shi Meiyun,Yin Lei
A sensitive UPLC-MS/MS method was developed and validated for quantifying polyethylene glycol 1000 (PEG1000) in zebrafish tissues, featuring a systematic comparison of two MS acquisition strategies. Through comprehensive optimization, the ammonium adduct [M+NH 4 ] + of the representative 18-EO oligomer ( m/z 828.5) was selected as the precursor ion, achieving approximately fourfold higher signal intensity than [M+H] + . Critically, the conventional high declustering potential in-source CID approach monitoring fragment ions was outperformed by the optimized MRM method monitoring the intact ammoniated precursor, which demonstrated 2.7-fold signal enhancement and superior selectivity. The integration of micro-solid-phase extraction (μ-SPE) further improved method performance, yielding 1.5-fold signal gain and markedly reduced matrix effects compared to conventional protein precipitation. The fully validated method exhibited excellent linearity (0.5–50 μg/mL, r > 0.995), accuracy, precision, and stability. Application to zebrafish tissue distribution studies revealed pronounced organ-specific accumulation following aqueous exposure to 200 μg/mL PEG1000, with highest concentrations in intestine tissue exhibiting a time-dependent increase, followed by muscle, while muscle maintained consistently low levels. This analytical platform, synergistically combining μ-SPE cleanup and ammoniated adduct-based MRM, offers superior sensitivity over in-source CID approaches and provides a practical framework for polymer bioanalysis, yielding critical insights into the in vivo fate of PEG-based compounds. The key novelties of this work are the following: (i) the first systematic comparison between ammoniated adduct MRM and high-DP in-source CID for PEG1000 quantification; (ii) the introduction of μ-SPE for sample preparation in zebrafish tissues, achieving 1.5-fold signal enhancement; and (iii) the successful application of this platform to reveal organ-specific accumulation patterns of PEG1000. Graphical abstract
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PubMed
高影响因子
Analytical Methods
·
2015
·Vol. 7
·期 9
·3876-3882
·
IF 1.821
Yamei Li,Limin Zhang,Huayun Han,Xiaoli Tian,Xinxin Shi,Kai Wang,Shusheng Zhang
A new modified silica gel with alizarin complexone has been prepared and proven to act as a promising adsorbent. Ultra trace Cu(II) and Cd(II) can be selectively enriched and separated from rice and water samples by solid phase extraction and detected by FAAS. What is more, 0.003 mol L−1 and 0.25 mol L−1 of HNO3 can be used as eluent for the gradient elution of Cd(II) and Cu(II), respectively. Cu(II) could be completely separated from Cd(II) and monitored with the naked eye using color agent 5-Br-PADAP. The selectivity of the adsorbent and the effects of solution pH, type and concentration of the eluent, and foreign ions have been investigated and optimized. Under the optimized conditions, the adsorption capacity for Cu(II) and Cd(II) was 0.511 and 0.157 mmol g−1, respectively. Determination of Cu(II) and Cd(II) by FAAS was linear in the range of 1.0–200 µg L−1 and 2.5–100 µg L−1 with a detection limit of 0.21 µg L−1 and 0.46 µg L−1, respectively. Comparing the determination results for Cu(II) and Cd(II) in water and rice using the new method with those detected by ICP-MS, a considerable difference was not observed between the two methods. The method was validated with the certified reference material GBW08511 rice. Moreover, the determination of Cu(II) in the range of 20–120 µg L−1 is sensitive to the naked eye and the determination results are good in agreement with those detected by UV-Visible spectrometry. The proposed method was simple and capable of determining Cu(II) and Cd(II) in real samples accurately.
研究领域:
分析化学
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环境科学
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DOI
高影响因子
FLAVOUR AND FRAGRANCE JOURNAL
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2021
·Vol. 37
·期 2
·83-95
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IF 2.576
Mingji Xiao,Fangling Zheng,Mengxuan Xiao,An Qi,Huiqiang Wang,Qianying Dai
In China, Lu'an Guapian (LAGP) tea consists of tea leaves without tea buds or stems. In this study, we evaluated the aromatic characteristics of LAGP by sensory analysis, aroma extract dilution analysis (AEDA), and odor activity values. The sensory analysis revealed that LAGP had cooked soybean-like, cooked chestnut-like, roasted, cooked corn-like, fishy, fruity, floral, and grass aromas. Aroma-active compounds from LAGP were identified by solvent extraction-solid phase extraction (SE-SPE) and headspace-solid phase microextraction (HS-SPME), and subjected to AEDA. A total of 91 aroma-active compounds were identified by SE-SPE-AEDA with flavor dilution (FD) factors ranging from 1 to 4096. A total of 66 aroma-active compounds were identified by HS-SPME-AEDA with FD of 1 to 128. Nine compounds with FD ≥64 and OAVs ≥1 were major aroma-active compounds to the aroma of LAGP tea: raspberry ketone (raspberry), ( E )- β -ionone (floral, raspberry), dimethyl sulfide (cooked corn-like), indole (animal), phenylacetaldehyde (floral, honey-like), 2-ethyl-3,5-dimethylpyrazine (roasted), ( Z )-4-heptenal (cooked soybean-like, fishy), ( Z )-jasmone (jasmine), and geraniol (rose).
研究领域:
食品科学
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农业化学
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分析化学
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茶叶科学
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）