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JOURNAL OF CHROMATOGRAPHY A · 2024 · IF 3.8

Ultrasound-assisted rapid growth of chemically bonded bifunctional mesoporous covalent organic framework submicrospheres on a nickel-chromium alloy support for efficient solid-phase microextraction of bisphenols from water and milk samples

Haixia Liu,Honghong Rao,Jinxin Guo,Baolan Lu,Yuyun Wang,Rongxi Zhu,Xinzhen Du

A layer-by-layer chemical bonding strategy was developed for fast in situ growth of bifunctional mesoporous covalent organic framework submicrospheres (COF SMSs) on the nickel-chromium alloy (Ni-Cr) fiber substrate via the ultrasound-assisted Schiff-base reaction for the first time. COF SMSs showed well-defined morphology, extraordinary high surface area (1211 m 2 · g −1 ) and narrow mesopore (2.50 nm) as well as excellent stability. Furthermore, the resulting Ni-Cr fiber presented outstanding adsorption capability and improved selectivity for bisphenols (BPs). Consequently, an attractive SPME-HPLC-UV approach with the Ni-Cr@Ni-Cr LDHs NSs@COF SMSs fiber was proposed for rapid preconcentration and sensitive determination of BPs. By optimizing adsorption parameters, the SPME-HPLC-UV method presented good linearity for five BPs in the ranges of 0.02–200 ng·mL −1 with coefficients of determination ( R 2 ) higher than 0.999. Limits of detection and limits of quantitation were obtained from 0.003 ng·mL −1 to 0.006 ng·mL −1 and from 0.010 to 0.019 ng·mL −1 , respectively. Moreover, the intra-day and inter-day precision expressed as relative standard deviations (RSDs) was 1.57–3.52 % and 2.65–4.38 % for the proposed method with a single fiber, respectively. RSDs of the proposed method with different duplicate fibers were 3.25–6.72 %. The proposed SPME-HPLC-UV method was available for efficient preconcentration and sensitive detection of five BPs from real water and milk samples. The relative recoveries at three spiking levels of BPs were achieved in the range of 80.00–118.8 % with RSDs below 7.81 %. In addition, the prepared fiber still exhibited satisfactory adsorption performance after 120 adsorption-desorption cycles.

研究领域: 分析化学 · 环境科学 · 材料科学
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CHROMATOGRAPHIA · 2013 ·Vol. 76 ·期 13 ·735-745 · IF 1.437

Study of Retention Mechanism of a Mixed-Mode Stationary Phase and Its Application for the Simultaneous Determination of Ten Water- and Fat-Soluble Vitamins by HPLC–UV

Peng Xi-Tian,Li Ze,Zhang Yi,Liu Tao,Yu Qiong-Wei,Feng Yu-Qi

A novel mixed-mode stationary phase (OAS) has been prepared by bonding n -octyl and aminopropyl groups with the surface of silica gel. The obtained OAS stationary phase was characterized by Fourier transform infrared spectroscopy, elemental analysis, zeta potential and ion-exchange capacity. The mixed-mode one-site and two-site retention models were used to quantitatively describe the retention mechanism of the OAS stationary phase using three strong acidic analytes. The results indicated that the two-site model is more suitable for the description of mechanism of OAS phase. Then the OAS stationary phase was applied to separate ten water- and fat-soluble vitamins in a single run; the separation is based on the hydrophobic and ionic interaction mechanisms. A method for the simultaneous determination of ten water- and fat-soluble vitamins in commercial multivitamin tablets by high performance liquid chromatography with ultraviolet detection was established and validated according to the stability, linearity, accuracy and precision. Finally, the validated method was used to analyze the content of ten vitamins in two commercial multivitamin tablets and the recoveries were in the range of 89.2–111.0 %, with RSDs <6.1 %, indicating the good reliability of the proposed method.

研究领域: 分析化学 · 药物分析
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Food Analytical Methods · 2026 ·Vol. 19 ·期 1 ·60 · IF 3

Magnetic Solid Phase Extraction of Five Sudan Dyes from Powdered Chili Pepper Samples Using C18/DVB/NVP-Multifunctional Core–Shell Magnetic Nanoparticles Followed by HPLC–UV Analysis

Hussain Aisha,Wu Jiapeng,Wen Jiaxi,Xiong Chaomei

Sudan dyes, a class of azo dyes, are genotoxic and carcinogenic to humans. However, they are still used illegally to color food products and spices due to their color fastness. In this study, multi-functionalized magnetic silica nanoparticles (C 18 /DVB/NVP(4:1)-Fe 3 O 4 @SiO 2 MNPs) were synthesized, and solid–liquid extraction (SLE) coupled with magnetic solid phase extraction (MSPE) was employed for the extraction and preconcentration of five Sudan dyes (Sudan I − IV, Sudan Red 7B), followed by high-performance liquid chromatography/ultraviolet spectroscopy (HPLC–UV) for their detection in powdered chili pepper samples. The SLE conditions for the analytes in powdered chili pepper samples were optimized. Under optimal conditions, the extraction recovery ranged between 78.0% and 106.9%. We investigated and optimized the potential factors that may affect the efficiency of MSPE. Under these optimal conditions, calibration curves showed good linearity ( R 2  > 0.9989) across the tested concentration range of 0.98 to 125 µg/g. The limits of detection for the five Sudan dyes were in the range of 0.06–0.26 µg/g. The intra-day and inter-day accuracy ranged from 93.5% to 106.3% with a relative standard deviation (RSD) of not more than 9.1%. The developed method was successfully applied to analyze ten different commercial brands of powdered chili pepper samples purchased from markets in Wuhan, confirming its feasibility for routine analysis of illegal Sudan dyes in these samples.

CAS / MDL: 10025-77-1 1321-74-0
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MICROCHEMICAL JOURNAL · 2023 · IF 4.8

Carboxyl-based deep eutectic solvent modified magnetic graphene oxide as a novel adsorbent for fast enrichment and extraction of estrogens in milk prior to HPLC-UV analysis

Yachao Hao,Wei Zhou,Xin Wang,Youping Liu,Xin Di

In this study, a magnetic graphene oxide modified with green carboxyl-based deep eutectic solvent (MGO@DES) was synthesized for the first time and employed as a highly efficient adsorbent for the magnetic solid-phase extraction (MSPE) of three estrogens in milk samples. With large specific surface, good hydrophobicity and abundant adsorption sites, MGO@DES exhibited excellent extraction performance for estrogens. The adsorption kinetic experiment revealed that 5 mg of MGO@DES reached the equilibrium of estrogen adsorption within 3 min. MGO@DES based MSPE coupled with HPLC-UV method was developed and applied to the determination of three estrogens in milk samples. Good linearity (R 2  > 0.9953) was obtained in the range of 1–200 ng mL −1 and the low limits of detection were 0.20–0.28 ng mL −1 . The spiked recoveries were in the range of 90.3–105.7%, with RSDs less than 7.9%.

CAS / MDL: 53-16-7 50-28-2 57-63-6
研究领域: 分析化学 · 环境科学
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FOOD CHEMISTRY · 2024 · IF 8.5

Fabrication of fluorinated magnetic microporous organic network for selective and efficient extraction of benzoylurea insecticides in tea beverages

Hui-Ping Yu,Qian-Qian Xu,Xin Wang,Yuan-Yuan Cui,He-Fang Wang,Cheng-Xiong Yang

In this work, a novel fluorinated magnetic microporous organic network (Fe 3 O 4 @FMON) was exquisitely designed and synthesized for highly efficient and selective magnetic solid phase extraction (MSPE) of fluorinated benzoylurea insecticides (BUs) from complex tea beverage samples. The Fe 3 O 4 @FMON exhibited good extraction for BUs via the pre-designed hydrophobic, π-π stacking, hydrogen bonding and specific F F interactions. A sensitive Fe 3 O 4 @FMON-based MSPE-HPLC-UV method with wide linear range (0.10–1000 μg L −1 , R 2  ≥ 0.996), low limits of detection (0.01–0.02 μg L −1 ), and large enrichment factors (85.6–98.0) for BUs from tea beverage samples was developed. By decorating F elements within MON's networks, the Fe 3 O 4 @FMON characterized good hydrophobicity and chemical stability, which could be reused at least 8 times without decrease of recoveries. This work demonstrated the great prospects of Fe 3 O 4 @FMON for enriching trace BUs from complex substrates and triggered the potential of FMON for sample pretreatment of fluorinated analytes.

研究领域: 分析化学 · 环境科学 · 材料科学 · 食品科学
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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
研究领域: 食品安全 · 分析化学 · 兽医药理学
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ANALYTICAL LETTERS · 2021 · IF 2.329

Reduced Graphene Oxide Nanoribbons for the Magnetic Solid-Phase Extraction (MSPE) of Bisphenol Endocrine Disruptors in Carbonated Beverages with Determination by High-Performance Liquid Chromatography with Ultraviolet Detection (HPLC-UV)

Ya-Wen Ding,Shi-Lan Feng,Juan Chen

A novel magnetic reduced graphene oxide nanoribbons (Fe3O4 @RGONRs) composite was prepared and applied as an adsorbent of magnetic solid-phase extraction (MSPE) for the determination of four bisphenol endocrine disrupters in three carbonated beverages coupled with high-performance liquid chromatography (HPLC). The prepared Fe3O4@RGONRs composite was characterized by transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, vibrating sample magnetometry, nitrogen adsorption-desorption isotherms and zeta potential analysis. Fe3O4@RGONRs composite possessed an abundant π-electron system and interacted with the analytes by π-π stacking, hydrophobic interactions, and hydrogen bond. The MSPE parameters, including the mass of adsorbent, sample solution pH, extraction time, ionic strength, desorption solvent and desorption time, were evaluated. Under the optimal conditions, the proposed Fe3O4@RGONRs-based MSPE method exhibited good linearity with determination coefficients (R2) between 0.9994 and 1000 from 1.6 to 1000 µg L−1, low limits of detection from 0.33 to 0.87 µg L−1, and suitable accuracy with spiked recoveries from 81.88% to 115.73%. The excellent analytical performance, along with suitable batch-to-batch reproducibility and reusability, suggest potential applications in the field of sample pretreatment.

CAS / MDL: 115-39-9 1478-61-1
研究领域: 分析化学 · 环境科学
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INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES · 2024 · IF 7.7

Multiple fingerprint and pattern recognition analysis on polysaccharides of four edible mushrooms

Shuangyu Shao,Xiali Si,Yingtao Zhang,Jun Li,Pengfei Tu,Qingying Zhang

Quality analysis of edible mushrooms based on polysaccharides is generally difficult due to their complicated structures and hard separation. Here, multiple fingerprint analysis of polysaccharides based on chromatographic and spectrometric techniques were developed, and then applied in comparative analysis of Auricularia heimuer (AH), Auricularia cornea (AC), Auricularia cornea ʻYu Muerʼ (ACY) and Tremella fuciformis (TF). Firstly, polysaccharides were obtained with the molecular weights between 1.783 × 10 6 and 6.774 × 10 6  Da. Then, complete hydrolysis by TFA and enzyme digestion by cellulase were employed and subsequently analyzed by HPLC-UV, GC–MS, HILIC-HPLC-ELSD and HILIC-HPLC-ESI − -HCD-MS/MS, and ATR-FT-IR were used to characterize the functional groups of intact polysaccharides. By chemometric analysis, differential markers of d -xyl, l -fuc, l -arb, d -glc, disaccharide and hexasaccharide were selected, and AC and ACY were proved to be same species from the viewpoint of polysaccharides firstly. Furthermore, the structures of oligomers with DPs of 2–8 and →4)- β - d -Glc p -(1→ unit with different contents were inferred by combinatory analysis of ESI − -MS/MS, glycosidic linkage, monosaccharide compositions and functional groups. In conclusion, the combinatory method of multiple fingerprint and pattern recognition is powerful not only for structural elucidation of polysaccharides, but also for quality analysis and species differentiation of edible mushrooms from the perspective of biological polysaccharides.

CAS / MDL: 89-25-8
研究领域: 食品科学 · 分析化学 · 真菌学 · 生物化学
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Journal of Functional Foods · 2016 · IF 3.973

Comparative analysis of multiple ingredients in Rosa roxburghii and R. sterilis fruits and their antioxidant activities

Jing-Yu He,Yuan-He Zhang,Na Ma,Xu-Lin Zhang,Meng-Hua Liu,Wei-Ming Fu

The functional and potential bioactive ingredients, including the elements, amino acids and phytochemicals, in Rosa roxburghii (RR) and R. sterilis (RS) fruits were analysed by ICP-OES and -MS, HPLC-UV, and LC-MS/MS, respectively, and were compared to elucidate the characteristics of their ingredients. The antioxidant activities of the ethanolic extracts of RR and RS fruits were evaluated using four different methods, including 2,2-diphenyl-1-picrylhydrazyl radical scavenging activity, hydroxyl radical scavenging activity, inhibition of β -carotene bleaching, and ferric reducing antioxidant power assays; the correlation between the ingredients and their antioxidant activities was assessed. Furthermore, principal component analysis was selected to differentiate between the intra- and interspecies variation of RR and RS fruits. The results showed that RR and RS fruits contained numerous nutritious and biological ingredients and exhibited antioxidant activities, but there were significant differences among the fruits. Nevertheless, RR and RS fruits are attractive materials to produce highly valuable, functional foods.

研究领域: 植物学 · 药理学 · 食品科学 · 分析化学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2021 · IF 7.312

Glycine betaine enhanced foam separation for recovering and enriching protein from the crude extract of perilla seed meal

Nan Hu,Keke Zhang,Yanfei Li,Tianyu Hou,Zhijun Zhang,Huizhen Li

The utilization of agro-food waste into protein products is an alternative solution for global protein shortage and waste management. Perilla ( Perilla frutescens L.) seed meal (PSM) is abundant and protein-rich by-products from the oilseed industry. To achieve the industrial production of valuable PSM protein (PSMP), a two-stage foam separation with a low cost and a high efficiency was developed to fractionate the high-concentration PSMP (1.3 times its critical micelle concentration (CMC)) from its crude extract. In the first-stage, glycine betaine (GB), a naturally occurring osmolyte, was used as a green enhancer for the recovery of PSMP. The result of SEM, FTIR, UV–vis and fluorescence spectra demonstrated that GB engaged in cation-π interactions with aromatic residues of PSMP, which made the protein structure unfold and enabled its hydrophobic groups of PSMP to be more exposed. These factors, plus protein aggregation, were responsible for the enhanced interfacial adsorption of PSMP. Its recovery percentage with 0.3 g/L GB (pH 7.0) increased by 52.9% compared to that without GB. Furthermore, an internal component of regular-hexagon hollow prismoid (RHP) was also designed to intensify the foam drainage and raise PSMP enrichment to 7.1 ± 0.3. In the second-stage, PSMP could be further recovered and its total recovery percentage reached 94.5 ± 4.7%. After foam separation, the amino acid composition of PSMP was analyzed by SDS-PAGE and HPLC–UV and its functional properties was also evaluated. These results provide a new insight into enhancing the protein separation from agro-food waste.

CAS / MDL: 6104-59-2
研究领域: 食品科学 · 蛋白质工程 · 废物管理 · 生物技术
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