Publications by authors named "Hongyuan Yan"

112 Publications

Defatted Seeds of as a Potential Functional Food Ingredient for Diabetes.

Foods 2021 Mar 5;10(3). Epub 2021 Mar 5.

Key Laboratory of Public Health Safety of Hebei Province, College of Public Health, Hebei University, Baoding 071002, China.

The defatted seeds of (DSOB) are a by-product of evening primrose oil production that are currently not effectively used. In this study, α-glucosidase inhibition, aldose reductase inhibition, antioxidant capacity, polyphenol composition, and nutritional value (carbohydrates, proteins, minerals, fat, organic acid, and tocopherols) of DSOB were evaluated using the seeds of (SOB) as a reference. DSOB was an excellent inhibitor of α-glucosidase (IC = 3.31 μg/mL) and aldose reductase (IC = 2.56 μg/mL). DSOB also showed considerable antioxidant capacities (scavenging of 2,2-diphenyl-1-picrylhydrazyl, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid, nitric oxide, peroxynitrite, and hydroxyl radicals). DSOB was a reservoir of polyphenols, and 25 compounds in DSOB were temporarily identified by liquid chromatography coupled with electrospray ionization-quadrupole time of flight-mass spectrometry analysis. Moreover, the carbohydrate, protein, and mineral content of DSOB were increased compared to that of SOB. DSOB contained large amounts of fiber and low levels of sugars, and was rich in calcium and iron. These results imply that DSOB may be a potential functional food ingredient for diabetes, providing excellent economic and environmental benefits.
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http://dx.doi.org/10.3390/foods10030538DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC8002154PMC
March 2021

Selective, sensitive, and miniaturized analytical method based on molecularly imprinted graphene oxide composites for the determination of naphthalene-derived plant growth regulators in apples.

Food Chem 2021 Jul 6;349:128982. Epub 2021 Jan 6.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis of Ministry of Education, College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China; Key Laboratory of Analytical Science and Technology of Hebei Province, Institute of Life Science and Green Development, Hebei University, Baoding 071002, China. Electronic address:

This paper reports a selective, sensitive, and miniaturized analytical method based on a molecularly imprinted graphene oxide (MIP-GO) composite as adsorbent for miniaturized tip solid-phase extraction (MTSPE) to determine naphthalene-derived plant growth regulators (PGRs) in apples. The proposed method combines the advantages of MIP-GOs (high selectivity), MTSPE (low consumption), and high-performance liquid chromatography-fluorescence detection (high sensitivity). Under optimized conditions, the method exhibited appreciable linearity (2.00-200 ng/g), low detection limits (0.21-0.53 ng/g), high accuracy (absolute recoveries: 87.6-99.5%), and high precision (relative standard deviations ≤ 3.0%), along with low consumption (0.5 mL sample solution and 2.0 mg adsorbent). In addition, the adsorption performance of the MIP-GO adsorbent did not decrease over ten months, highlighting the long storage and operational lifetime of the adsorbent. The proposed method was employed for the analysis of naphthalene-derived PGR residues in apples and exhibited promising potential for application in food safety analysis.
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http://dx.doi.org/10.1016/j.foodchem.2020.128982DOI Listing
July 2021

MOF-74@SiO core-shell stationary phase: Preparation and its applications for mixed-mode chromatographic separation.

J Chromatogr B Analyt Technol Biomed Life Sci 2021 Jan 19;1163:122506. Epub 2020 Dec 19.

College of Pharmaceutical Sciences, Key Laboratory of Public Health Safety of Hebei Province, Hebei University, Baoding 071002, China; Key Laboratory of Medicinal Chemistry and Molecular Diagnosis of Ministry of Education, Institute of Life Science and Green Development, Hebei University, Baoding 071002, China. Electronic address:

The development of versatile mixed-mode stationary phase materials is of important meanings for solving the increasing demands for real sample analysis. Herein, with 2,5-dihydroxyterephthalic acid as the organic ligand and nickel as the metal centre, MOF-74 nanocrystal materials were facilely grafted on the surface of carboxyl-functionalized silica gel via layer-by-layer assembling technique. The structures of the monodisperse MOF-74@SiO material were proved by Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, elemental analysis, thermogravimetric analysis, and Brunauer-Emmett-Teller specific surface area and pore size analyzer, respectively. Because the introduced 2,5-dihydroxyterephthalic acid is of hydrophilic carboxyl and hydroxyl groups, the packed MOF-74@SiO column reveals hydrophilic interaction/reversed-phase mixed-mode retention properties. Compared with commercial C column or silica-based column, the MOF-74@SiO column shows distrinct separation selectivity in short separation time for polycyclic aromatic hydrocarbons, phenolic compounds and polar sulfonamide compounds. The developed MOF-74@SiO column was further successfully applied for the separation and detection of illegal addition of glucocorticoid in children's face cream as well as sulfonamides veterinary drug residues in pure milk. The research provides a simple and convenient approach to prepare multifunctional MOFs-based stationary phase materials.
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http://dx.doi.org/10.1016/j.jchromb.2020.122506DOI Listing
January 2021

Recent Applications of Carbon Nanomaterials for microRNA Electrochemical Sensing.

Chem Asian J 2021 Jan 18;16(2):114-128. Epub 2020 Dec 18.

College of Pharmaceutical Science, Hebei University Institute of Life Science and Green Development, Key Laboratory of Pharmaceutical Quality Control of Hebei Province, Baoding, 071002, P. R. China.

MicroRNA (miRNA) is an important tumor marker in the human body, and its early detection has a great influence on the survival rate of patients. Although there are many detection methods for miRNA at present such as northern blotting, real-time quantitative polymerase chain reaction, microarrays, and others, electrochemical biosensors have the advantages of low detection cost, small instrument size, simple operation, non-invasive detection and low consumption of reagents and solvents, and thus they play an important role in the early detection of cancer. In addition, with the development of nanotechnology, nano-biosensors show great potential. The application of various nanomaterials in the development of electrochemical biosensor has greatly improved the detection sensitivity of electrochemical biosensor. Among them, carbon nanomaterials which have unique electrical, optical, physical and chemical properties have attracted increasing attention. In particular, they have a large surface area, good biocompatibility and conductivity. Therefore, carbon nanomaterials combined with electrochemical methods can be used to detect miRNA quickly, easily and sensitively. In this review, we systematically review recent applications of different carbon nanomaterials (carbon nanotubes, graphene and its derivatives, graphitic carbon nitride, carbon dots, graphene quantum dots and other carbon nanomaterials) for miRNA electrochemical detection. In addition, we demonstrate the future prospects of electrochemical biosensors modified by carbon nanomaterials for the detection of miRNAs, and some suggestions for their development in the near future.
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http://dx.doi.org/10.1002/asia.202001260DOI Listing
January 2021

An integrated solid phase extraction with ionic liquid-thiol-graphene oxide as adsorbent for rapid isolation of fipronil residual in chicken eggs.

J Chromatogr A 2020 Sep 19;1631:461568. Epub 2020 Sep 19.

Key Laboratory of Public Health Safety of Hebei Province, College of Public Health, Hebei University, Baoding, 071002, China. Electronic address:

A rapid and economic integrated solid-phase extraction (ISPE) method with ionic liquid-thiol-graphene oxide composite (IL-TGO) as a new adsorbent was established for the extraction of fipronil in chicken eggs. In this study, ISPE, a new form of solid-phase extraction, which combined the advantages of pipette-tip solid phase extraction (PT-SPE) and dispersive solid-phase extraction (DSPE), achieving rapid extraction of analyte with only a small amount of adsorbent. The three-dimensional porous IL-TGO was a new ideal adsorbent for fipronil due to the multiple adsorption interactions (π-π interaction, hydrophobic interaction and hydrogen bond), large adsorption capacity and fast adsorption rate. For this ISPE procedure, the analyte was adsorbed by IL-TGO through the pipette tip mode and then eluted through dispersive mode. Under the optimized condition, the proposed method performed following merits: good linearity (r = 0.9999), precision (RSD ≤ 6.3%), high recoveries (83.7% to 97.7%), rapid extraction (16 min), low consumption of adsorbent (3.00 mg of IL-TGO). The excellent recyclability of the ISPE device and the reusability of IL-TGO were observed and high recovery of fipronil (> 90%) was obtained after fifteen cycles. This work might provide promising strategy for the sensitive extraction and analysis of trace levels of fipronil from egg products.
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http://dx.doi.org/10.1016/j.chroma.2020.461568DOI Listing
September 2020

On-line enrichment and determination of aristolochic acid in medicinal plants using a MOF-based composite monolith as adsorbent.

J Chromatogr B Analyt Technol Biomed Life Sci 2020 Nov 28;1159:122343. Epub 2020 Aug 28.

Key Laboratory of Public Health Safety of Hebei Province, College of Pharmacy, Hebei University, Baoding, 071002, China, Key Laboratory of Medicinal Chemistry and Molecular Diagnosis of Ministry of Education, Institute of Life Science and Green Development, Hebei University, Baoding 071002, China. Electronic address:

In this study, modified UiO-66-NH and N-methylolacrylamide (NMA) were used as common monomers to prepare a metal organic framework (MOF)-based composite monolith through in-situ polymerization, which was used as a new adsorbent to purify and enrich aristolochic acid-I (AA-I) in medicinal plants. The MOF-based composite monolithic column was characterized by nitrogen adsorption-desorption isotherm, mercury intrusion porosimetry and scanning electron microscopy (SEM). The adsorption ability of MOF-based composite monolith for AA-I was compared with that of the polymer monolith without MOF added. The results proved that the addition of UiO-66-NH can increase both the specific surface area and the permeability of the monolith. Moreover, the adsorption amount of AA-I on the monolith improved. This proposed on-line solid phase extraction (SPE) method showed good linear relationship in the range 0.044 ~ 400 μg/mL with r = 0.9994; the limit of detection (LOD) was 13.08 ng/mL and the limit of quantification (LOQ) was 44.00 ng/mL; the intra-day and inter-day accuracies were less than 0.97%; the inter-column accuracies was less than 6.11%; the recovery was in the range of 91.11%~106.48%. The method was found to be easy, accurate and convenient for on-line enrichment and purification of AA-I in medicinal plants.
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http://dx.doi.org/10.1016/j.jchromb.2020.122343DOI Listing
November 2020

Application of a titanium-based metal-organic framework to protein kinase activity detection and inhibitor screening.

Anal Chim Acta 2020 Sep 11;1128:99-106. Epub 2020 Jul 11.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, College of Chemistry and Environmental Science, Hebei University, Baoding, 071002, China; College of Public Health, Institute of Life Science and Green Development, Hebei University, Baoding, 071002, China. Electronic address:

In this work, we used a titanium-based metal-organic framework (MOF, Ti-MIL125-NH) as a novel enrichment platform to detect protein kinase A (PKA) activity and to screen relevant kinase inhibitors. This method took advantage of the highly specific recognition of phosphate groups by the Ti-MIL125-NH nanoparticle. In the presence of PKA and adenosine 5'-triphosphate (ATP), the fluorophore-labeled peptide substrate was phosphorylated, and the generated phosphopeptide could then specifically bind to the titanium sites of Ti-MIL125-NH. This resulted in fluorescence enrichment, which could be efficiently detected by the system. Under optimal conditions, the method presented a linear relationship in the experimental range of 0.00005-0.01 U μL, and the limit of detection was 0.00003 U μL (3σ, n = 11). Furthermore, protein kinase Akt1 was tested to verify the universality of this method. The method was also successfully applied in cell lysates for kinase activity analysis and inhibitor screening. Thus, the new, highly sensitive fluorescence method based on MOF for detecting PKA activity is an excellent tool that has potential applications in kinase-related disease and basic research.
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http://dx.doi.org/10.1016/j.aca.2020.06.065DOI Listing
September 2020

Efficient enrichment and analysis of atrazine and its degradation products in Chinese Yam using accelerated solvent extraction and pipette tip solid-phase extraction followed by UPLC-DAD.

Food Chem 2021 Feb 4;337:127752. Epub 2020 Aug 4.

College of Chemistry and Environmental Science, Key Laboratory of Analytical Science and Technology of Hebei Province Hebei University, Baoding 071002, China.

The Chinese Yam (Dioscorea opposita) is cultivated widely in China. However, there are potential safety risks associated with herbicide residues in Chinese Yam because of its characteristics and unregulated use of pesticides. We developed an efficient sample preparation technique for simultaneous analysis of atrazine and its degradation products in Chinese Yam using accelerated solvent extraction and pipette tip solid-phase extraction followed by UPLC-DAD analysis. Molecularly imprinted polymer (MIP) were used as the adsorbent material. Method performance was evaluated and our results showed the limit of quantification was 1-3 μg/ kg, with recoveries in the range 79.2-103.8%. When compared with other methods, this method provided superior performance in terms of sensitivity, accuracy, and precision. This method is, therefore, expected to be useful in supervised residue analysis.
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http://dx.doi.org/10.1016/j.foodchem.2020.127752DOI Listing
February 2021

Surface Siloxane-Modified Silica Materials Combined with Metal-Organic Frameworks as Novel MALDI Matrixes for the Detection of Low-MW Compounds.

ACS Appl Mater Interfaces 2020 Aug 4;12(33):37793-37803. Epub 2020 Aug 4.

Tianjin Key Laboratory of Risk Assessment and Control Technology for Environment and Food Safety, Tianjin Institute of Environmental and Operational Medicine, Tianjin 300050, China.

Surface siloxane (3-aminopropyl triethoxysilane hydrolyzates)-modified silica materials were used as "initiators", which resulted in the release and desorption of intact molecules adsorbed on the surface of a matrix. A covalently cross-linked MIL-53(Al) material was used to enhance the ionization of analytes. Herein, we have provided an efficient matrix-assisted laser desorption/ionization mass spectrometry (MALDI-TOF MS) matrix strategy, which responded to both ion and laser irradiation with low background interference in the low-molecular-weight (MW) region. The matrixes MIL-53(Al), SBA-15@APTES, SiO@APTES, SBA-15@APTES@MOF, and SiO@APTES@MOF were synthetized and used for the analysis of a series of low-MW compounds to verify the effectiveness of the strategies. Compared to conventional matrixes, the surface-modified SBA-15@APTES@MOF and SiO@APTES@MOF had low background, high sensitivity, extensive applicability, good stability, and ultrahigh tolerance of salt concentrations. The detection limits of standard analytes were determined to range from 0.1 to 1 × 10 mg/mL for 16 amino acids as well as citric acid, reserpine, tetraethylammonium chloride, melamine, bisphenol A, and malachite green. These results could help in designing more efficient nanostructure-initiator materials and further promote the application of MALDI-TOF MS.
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http://dx.doi.org/10.1021/acsami.0c11404DOI Listing
August 2020

Improved Solid-Phase Extraction for Simple, Sensitive, and Efficient Determination of Trace Plant Growth Regulators in Cherry Tomatoes by High-Performance Liquid Chromatography.

J Agric Food Chem 2020 Aug 24;68(31):8447-8454. Epub 2020 Jul 24.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis of Ministry of Education, College of Chemistry and Environmental Science, Hebei University, Baoding, Hebei 071002, People's Republic of China.

The overuse of plant growth regulators (PGRs) in agricultural products has gradually increased in recent years, resulting in hazardous effects on food safety and human health. For the first time, a sensitive, accurate, and low-cost analytical method involving improved solid-phase extraction coupled with high-performance liquid chromatography was developed to determine trace PGRs in cherry tomatoes. Thereafter, the extraction mechanism and conditions were elucidated. Under optimized conditions, good linearity (0.04-400 ng g; ≥ 0.9996) and lower limits of detection (0.005-0.006 ng g) were observed. The recoveries were 81.4-90.1%, with relative standard deviations of ≤6.7% (three levels). Finally, the developed method was successfully used to detect trace PGRs in cherry tomatoes. The results illustrated that this sensitive method shows great potential for application to monitor trace PGRs in agricultural products and, thus, provide technical support for food safety and public health.
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http://dx.doi.org/10.1021/acs.jafc.0c02636DOI Listing
August 2020

Deep eutectic solvent functionalized graphene oxide composite adsorbent for miniaturized pipette-tip solid-phase extraction of toluene and xylene exposure biomarkers in urine prior to their determination with HPLC-UV.

Mikrochim Acta 2020 06 14;187(7):387. Epub 2020 Jun 14.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, College of Public Health, Institute of Life Science and Green Development, Hebei University, Baoding, 071002, China.

A deep eutectic solvent functionalized graphene oxide composite adsorbent (DFG) was synthesized through reversible-addition fragmentation chain-transfer polymerization. The synthesized DFG had multiple adsorption interactions after covalent modification with a deep eutectic solvent (allyltriethylammonium bromide/ethylene glycol). Adsorption isotherms and kinetics studies of DFG indicate that the adsorption of hippuric acid (HA) and methylhippuric acid (MHA) was monolayer chemical adsorption. The comparison of DFG with commercial adsorbents demonstrates that the adsorption ability of DFG was superior. This was due to the multiple adsorption interactions of DFG for the three analytes (mainly π-interaction, hydrogen bonding, electrostatic adsorption, and hydrophobic interaction). The DFG adsorbent was applied to miniaturized pipette-tip solid-phase extraction (MPT-SPE), followed by high-performance liquid chromatography (HPLC) to determine biomarkers in urine for toluene and xylene exposure. The DFG-MPT-SPE-HPLC method required only 2.00 mg of DFG as adsorbent, 0.50 mL of washing solvent, and 0.40 mL of elution solvent to achieve a wide linear range (0.200-200 μg mL), high recoveries (90.9-99.1%), and high precision (RSD ≤ 6.3%). The proposed method was applied to determine HA and MHA in urine samples from occupational workers. Graphical abstract Deep eutectic solvent functionalized graphene oxide composite adsorbent for miniaturized pipette-tip solid-phase extraction of toluene and xylene exposure biomarkers in urine prior to their determination with HPLC-UV.
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http://dx.doi.org/10.1007/s00604-020-04370-zDOI Listing
June 2020

Imidazolium ionic-liquid-modified phenolic resin for solid-phase extraction of thidiazuron and forchlorfenuron from cucumbers.

J Chromatogr A 2020 Jul 5;1623:461192. Epub 2020 May 5.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, College of Public Health, Hebei University, Baoding, 071002, China; Key Laboratory of Analytical Science and Technology of Hebei Province, College of Pharmaceutical Science, Hebei University, Baoding, 071002, China. Electronic address:

An imidazolium ionic-liquid-modified phenolic resin (ILPR) was synthesized using 3-aminophenol as a functional monomer, glyoxylic acid as a green cross-linker, and polyethylene glycol 6000 as a porogen. The obtained ILPR showed better extraction of benzoylurea plant hormones thidiazuron and forchlorfenuron than the unmodified phenolic resin because the imidazolium IL provides more interaction modes with the analytes. ILPR, as a tailored adsorbent for solid-phase extraction, was coupled with high-performance liquid chromatography (ILPR‒SPE‒HPLC) for the simultaneous determination of thidiazuron and forchlorfenuron in cucumbers. Good linearity of the ILPR‒SPE‒HPLC method was obtained, ranging from 0.0100 to 5.00 μg g with a correlation coefficient (r) ≥ 0.9999. The recoveries of spiked samples ranged from 91.4% to 100.7% with a relative standard deviation of ≤ 6.0%.
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http://dx.doi.org/10.1016/j.chroma.2020.461192DOI Listing
July 2020

One pot green synthesis of m-aminophenol-urea-glyoxal resin as pipette tip solid-phase extraction adsorbent for simultaneous determination of four plant hormones in watermelon juice.

J Chromatogr A 2020 Jul 8;1623:461214. Epub 2020 May 8.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis of Ministry of Education, College of Public Health, Hebei University, Baoding 071002, China; Key Laboratory of Analytical Science and Technology of Hebei Province, College of pharmacy, Hebei University, Baoding 071002, China. Electronic address:

Plant hormones (PHs) are a type of pesticide that can potentially affect human health. Therefore, their quantitative detection is particularly important. In this study, a green and economic method for the simultaneous extraction and determination of four PHs, namely thidiazuron, forchlorfenuron, 1-naphthylacetic acid, and 2-naphthoxyacetic acid, in watermelon juice was developed by using m-aminophenol-urea-glyoxal resin as the adsorbent for pipette tip solid phase extraction (PT-SPE) coupled with liquid chromatography. The resin was synthesized via a simple (one pot hydrothermal synthesis) and green (ethanol as the solvent and glyoxal as crosslinking agent) process. The synthesized resin possesses multiple functional groups (hydroxyl, amino, and imino, among others), high adsorption capacity, larger specific surface area than the urea-glyoxal resin and m-aminophenol-glyoxal resin, and can be regenerated easily. The PT-SPE device is simple, cheap, and easy to obtain, and the adsorbent dosage is only 5.0 mg. The proposed method has a wide linear detection range, high recovery, good precision, and high sensitivity, and satisfies the measurement requirements for detecting trace levels of PHs in fruits and vegetables.
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http://dx.doi.org/10.1016/j.chroma.2020.461214DOI Listing
July 2020

Molybdenum disulfide-hypercrosslinked polymer composite as an adsorbent for determination of polycyclic aromatic hydrocarbons in environmental water coupled with HPLC-FLD.

Mikrochim Acta 2020 03 23;187(4):242. Epub 2020 Mar 23.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education & College of Public Health, Hebei University, Baoding, 071002, China.

A composite was synthesized from two-dimensional molybdenum disulfide (MoS) nanosheets and hypercrosslinked polymers (HCP), and the composite was characterized by infrared spectroscopy, scanning electron microscopy, and specific surface area. The fluffy and porous structure and multiple adsorption sites (π-interaction, static electricity, hydrogen bonding) make it ideal for use as an adsorbent. A pipette tip solid-phase extraction with the composite as the adsorbent combined with HPLC-FLD was developed to determine trace amounts of polycyclic aromatic hydrocarbons (phenanthrene, anthracene, fluoranthene, pyrene, benzo(α)anthracene) in environmental water. Under optimal extraction conditions, the method has a wide linear range (0.5-100 ng mL) and low limit of detection (0.024-0.099 ng mL), and the recoveries of PAHs from spiked environmental water were 73.8% to 123.6% (relative standard deviation ≤ 6.7%, n = 3). Graphical abstract Schematic representation of a three-dimensional molybdenum disulfide-ethylenediamine-hypercrosslinked polymer composite (MoS-EDA-HCP) using pipette tip solid-phase extraction adsorbent for extracting trace levels of polycyclic aromatic hydrocarbons (PAHs) prior to HPLC-FLD. HCP, hypercrosslinked polymer; MoS, molybdenum disulfide; EDA, ethylenediamine.
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http://dx.doi.org/10.1007/s00604-020-4220-0DOI Listing
March 2020

Selective extraction and detection of β-agonists in swine urine for monitoring illegal use in livestock breeding.

Food Chem 2020 May 7;313:126155. Epub 2020 Jan 7.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China; Key Laboratory of Analytical Science and Technology of Hebei Province, College of Public Health, Hebei University, Baoding 071002, China. Electronic address:

The illegal use of β-agonists often endangers animal-derived food safety. In this study, a selective detection method for β-agonists in swine urine was established via the combination of polymeric ionic liquid-molecularly imprinted graphene oxide-miniaturized pipette tip solid-phase extraction and high-performance liquid chromatography. It is worth noting that this method relied mainly on the designed adsorbent, which presented a rich adsorption mechanism, fast mass transfer rate, and high selectivity, and was successfully utilized in the selective extraction of β-agonists from swine urine samples. The proposed method has low LOD (0.20-0.56 ng/mL), high recovery (94.9-107.9%), and high reusability (4 times, 91.9-108.8%), which indicates its high potential as a selective, sensitive, accurate, and nonfatal method for monitoring the illegal use of β-agonists in the livestock breeding stage.
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http://dx.doi.org/10.1016/j.foodchem.2019.126155DOI Listing
May 2020

Fabrication of a cycloalkyl-monolith for on-line solid-phase extraction and determination of four polyphyllins in plasma.

Anal Biochem 2020 02 23;591:113555. Epub 2019 Dec 23.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, Hebei University, China.

A cycloalkyl-based polymer monolithic column for solid-phase extraction was prepared via radical polymerization using cyclohexyl methacrylate as the monomer. The preparative conditions such as crosslinker/monomer ratio and the amount of the porogens were optimized and the resulting monoliths were characterized by scanning electron microscopy and nitrogen adsorption-desorption method. On-line solid-phase extraction-high-performance liquid chromatography was performed to quantitatively analyse polyphyllin I, II, VI and VII contained in herbal medicine of paridis rhizome in mouse plasma using the homemade optimized monolithic SPE column combined with a C18 column, in which water was used to remove the plasma matrix while the polyphyllins in the mouse plasma were eluted by acetonitrile-water (42:58, V/V). Results obtained from the method validation show that the present method is feasible for the quantitative analysis of the four polyphyllins in plasma. The developed method was further applied for the real mouse plasma sample. These results show that the homemade cycloalkyl-based polymer monolithic SPE column has good ability for clean-up of the interfering bio-matrix and simultaneously extracting the four polyphyllins from mouse plasma. Furthermore, the present method is a promising method for quantitative determination of saponins compounds from complex bio-samples with the advantages of simple and efficient.
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http://dx.doi.org/10.1016/j.ab.2019.113555DOI Listing
February 2020

Newly designed molecularly imprinted 3-aminophenol-glyoxal-urea resin as hydrophilic solid-phase extraction sorbent for specific simultaneous determination of three plant growth regulators in green bell peppers.

Food Chem 2020 May 10;311:125999. Epub 2019 Dec 10.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, College of Public Health, Hebei University, Baoding 071002, China; Key Laboratory of Analytical Science and Technology of Hebei Province, College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China. Electronic address:

A method based on solid-phase extraction (SPE) coupled with high-performance liquid chromatography (HPLC) was developed to determine the content of 4-chlorophenoxy acetic acid (PCPA), naphthylacetic acid (NAA) and 2,4-dichlorophenoxyacetic acid (2,4-D) in green bell peppers. A molecularly imprinted 3-aminophenol-glyoxal-urea resin (MIAGUR) was first synthesized as a specific SPE adsorbent, which exhibited special selectivity and multiple adsorption interactions including hydrogen bonding and π-π interactions. The quantities of PCPA, NAA and 2,4-D in green bell peppers from 20 samples scattered throughout Baoding city (Hebei province, China) were determined using the proposed method. The results suggested that the use of PCPA, NAA and 2,4-D in green bell peppers from Baoding's markets is almost in fair. Moreover, MIAGUR-SPE-HPLC is suitable for the specific simultaneous monitoring of PCPA, NAA, and 2,4-D in green bell peppers and has potential applications in determination of PCPA, NAA, and 2,4-D of other plant products.
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http://dx.doi.org/10.1016/j.foodchem.2019.125999DOI Listing
May 2020

Ionic liquid-organic-functionalized ordered mesoporous silica-integrated dispersive solid-phase extraction for determination of plant growth regulators in fresh Panax ginseng.

Talanta 2020 Jan 9;207:120247. Epub 2019 Aug 9.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, College of Public Health, Hebei University, Baoding, 071002, China; Key Laboratory of Analytical Science and Technology of Hebei Province, College of Chemistry and Environmental Science, Hebei University, Baoding, 071002, China. Electronic address:

The massive accumulation of plant growth regulators (PGRs) in Panax ginseng causes serious harm to human health. A new analytical method for the simultaneous determination of multiple PGRs in 19 types of fresh Panax ginseng is developed by a new designed wool cluster-inspired ionic liquid-functionalized ordered mesoporous silica-integrated dispersive solid-phase extraction coupled to high performance liquid chromatography (IL-WFOMS-I-DSPE-HPLC). The proposed method combines the advantages of the multiple adsorption mechanisms, high mass transfer rate and large adsorption capacity of the synthesized IL-WFOMS adsorbent with the safe, convenient operation of the new designed I-DSPE method. Under optimized conditions, the recoveries at three spike levels were in a range of 77.6-98.3% for 3-indole acetic acid (IAA), 3-indole propionic acid (IPA), 3-indole butyric acid (IBA), and 1-naphthaleneacetic acid (NAA) with the relative standard deviations (RSD) ≤8.6%, n = 3. This method exhibits the advantages of safety, convenience, reliability, and has great potential for simultaneous determination of multiple trace PGRs in complex sample matrices.
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http://dx.doi.org/10.1016/j.talanta.2019.120247DOI Listing
January 2020

Simple quantitative analytical methods for the determination of alkaloids from medicinal and edible plant foods using a homemade chromatographic monolithic column.

J Chromatogr B Analyt Technol Biomed Life Sci 2019 Oct 4;1128:121784. Epub 2019 Sep 4.

College of Pharmaceutical Sciences, Hebei University, China; Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, Hebei University, China.

A polymer-based chromatographic monolithic column was prepared via in-situ radical polymerization using tetrahydrofurfuryl methacrylate as the monomer. The homemade column was used for the separation and quantitative analysis of alkaloids, including piperine from Piper longum (fruit of Piper longum Linn.) and pepper (fruit of Piper nigrum L.), hydroxy-α-sanshool, and hydroxy-γ-sanshool from zanthoxylum (fruit of Zanthoxylum bungeanum Maxim), as well as caffeine from Wuyi rock tea. The chromatographic fractions were identified by mass spectrometry. Single factor test and orthogonal test were both carried out to optimize the extraction conditions. The method validation indicated that the accuracy represented by spiked recovery ranged in 98.89%-102.06%, the correlation coefficients in 0.99986-0.99999. These results show that the prepared monolithic column can be successfully used to quantitatively analyse alkaloids from the real medicinal and edible plant foods with reversed-phase mechanism, which can avoid the long analytical time using traditional packed C18 column. The present method is a simple, and inexpensive method for quantitatively analysing alkaloids from medicinal and edible plant foods, exhibiting good specificity and durability.
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http://dx.doi.org/10.1016/j.jchromb.2019.121784DOI Listing
October 2019

Screening and Isolating Major Aldose Reductase Inhibitors from the Seeds of Evening Primrose ().

Molecules 2019 Jul 25;24(15). Epub 2019 Jul 25.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education & College of Public Health, Hebei University, Baoding 071002, China.

Aldose reductase (AR) is a drug target for therapies to treat complications caused by diabetes mellitus, and the development of effective AR inhibitors (ARIs) of natural origin is considered to be an attractive option for reducing these complications. In this research, the rat lens AR (RLAR) inhibitory activity of evening primrose () seeds was investigated for the first time. In our results, the 50% (/) methanol extract of evening primrose seeds exhibits excellent RLAR inhibitory activity (IC value of 7.53 μg/mL). Moreover, after enrichment of its bioactive components, the ARIs are more likely to be present in the ethyl acetate fraction of 50% () methanol extract (EME) of evening primrose seeds, which exhibits superior RLAR inhibitory activity (IC value of 3.08 µg/mL). Finally, gallic acid (), procyanidin B3 (), catechin (), and methyl gallate () were identified as the major ARIs from the EME by affinity-based ultrafiltration-high-performance liquid chromatography and were isolated by high speed countercurrent chromatography, with gallic acid (11.46 µmol/L) and catechin (14.78 µmol/L) being the more potent inhibitors of the four ARIs identified. The results demonstrated that evening primrose seeds may be a potent ingredient of ARIs.
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http://dx.doi.org/10.3390/molecules24152709DOI Listing
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC6695788PMC
July 2019

A metal organic framework polymer monolithic column as a novel adsorbent for on-line solid phase extraction and determination of ursolic acid in Chinese herbal medicine.

J Chromatogr B Analyt Technol Biomed Life Sci 2019 Sep 9;1125:121715. Epub 2019 Jul 9.

Key Laboratory of Pharmaceutical Quality Control of Hebei Province, College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China; Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, Baoding 071002, China.

A metal organic framework (MOF)-polymer monolithic column was prepared by redox initiation using modified MOF and N-methylolacrylamide (NMA) as co-monomers. The obtained monolithic column was characterized by scanning electron microscopy (SEM) and nitrogen adsorption-desorption isotherm measurement. It was used as a solid phase extraction (SPE) absorbent for the online enrichment of ursolic acid (UA) by high performance liquid chromatography. The adsorption amount of UA on the monolith was compared with that of silica gel-C18 adsorbent and the monolith without MOF material. The MOF-polymer monolithic column showed high selectivity and good permeability. Under the optimum conditions for extraction and determination, the calibration equation was y = 79.854× + 0.1939; the linear range was 0.001-0.9 mg/mL; the linear regression coefficient was 0.9993; the limit of detection (LOD) and the limit of quantification (LOQ) were 0.17 μg/mL and 0.57 μg/mL, respectively; the inter-day and intra-day accuracies were <6.44%; the recovery was in the range of 86.52-105.26%. The MOF-polymer monolithic column was successfully used as SPE column for enrichment and determination of UA in Chinese herbal medicine.
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http://dx.doi.org/10.1016/j.jchromb.2019.121715DOI Listing
September 2019

Attapulgite/hydrophilic molecularly imprinted monolithic resin composite for the selective recognition and sensitive determination of plant growth regulators in cucumbers.

Food Chem 2019 Nov 10;297:124974. Epub 2019 Jun 10.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, College of Public Health, Hebei University, Baoding 071002, China; Key Laboratory of Analytical Science and Technology of Hebei Province & College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China. Electronic address:

In this study, through in-situ polymerization process, a novel composite of attapulgite/hydrophilic molecularly imprinted monolithic resin (AT/HMIMR) were prepared in pipette tips for extraction trace plant growth regulators in cucumbers. In the preparation procedure, fibrillar attapulgite nanoparticles were embedded to increase extraction capacity, polyethyleneglycol-6000 was employed as a dual-function porogen, that acted as both the structure-directing agent of the HMIMR and the attapulgite dispersant. N-(1-naphthyl) ethylenediamine dihydrochloride was used as a dummy template to accurate quantification on extraction procedures. Experimental parameters of AT/HMIMR for extracting plant growth regulators from cucumbers were optimized, and the results showed that the recoveries of ranged from 92.4% to 101.1% with relative standard deviations ≤ 6.5% (n = 3). Considering its microporous monolithic column structure, multiple adsorption mechanism, and specific selectivity, AT/HMIMR shows promise for applications that require specific recognition for the analytes in real complex samples.
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http://dx.doi.org/10.1016/j.foodchem.2019.124974DOI Listing
November 2019

Cauliflower-like resin microspheres with tuneable surface roughness as solid-phase extraction adsorbent for efficient extraction and determination of plant growth regulators in cucumbers.

Food Chem 2019 Oct 20;295:259-266. Epub 2019 May 20.

Key Laboratory of Analytical Science and Technology of Hebei Province, College of Chemistry and Environmental Science, Hebei University, Baoding 071002, China. Electronic address:

New cauliflower-like phloroglucinol-glyoxylic acid resin microspheres (PGRMs) with controllable diameters and tuneable surface roughness were prepared using a one-step environmentally-friendly method without a catalyst. The PGRMs obtained exhibited a rough surface, narrow size distribution, and excellent adsorption capacity for polar compounds. The PGRMs were employed as an adsorbent for solid phase extraction (SPE) of kinetin (KT) and 6-benzyladenine (6-BA) in cucumbers and demonstrated better extraction recoveries and purification efficiency than phloroglucin-formaldehyde resin and common commercial adsorbents. Our PGRMs-SPE-HPLC method showed good linearity (r ≥ 0.9997) ranging from 0.04 to 4.00 μg/g for KT and 6-BA, and recoveries at three spiked concentration ranged from 77.8% to 104.4% with RSDs ≤ 6.8%. This PGRMs-SPE-HPLC method was applied successfully to determine of KT and 6-BA in cucumbers.
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http://dx.doi.org/10.1016/j.foodchem.2019.05.130DOI Listing
October 2019

Chiral Separation by NACE Using Polyol Derivative-Boric Acid Complexes.

Methods Mol Biol 2019 ;1985:383-389

Key Laboratory of Medical Chemistry and Molecular Diagnosis, Ministry of Education, Hebei University, Baoding, China.

Nonaqueous capillary electrophoresis (NACE) is an effective method for chiral separation. Many polyol derivatives (e.g., D-(+)-xylose, lactobionic acid, diacetone-D-mannitol, L-sorbose, and D-gluconic acid δ-lactone) can react with boric acid in methanol to produce polyol derivative-boric acid complexes which can be utilized as chiral selectors of enantioseparations. The enantiomers of more than a dozen basic analytes can be resolved under the optimized NACE using these chiral selectors.
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http://dx.doi.org/10.1007/978-1-4939-9438-0_22DOI Listing
January 2020

Graphene/multi-walled carbon nanotubes as an adsorbent for pipette-tip solid-phase extraction for the determination of 17β-estradiol in milk products.

J Chromatogr A 2019 Aug 22;1600:73-79. Epub 2019 Apr 22.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, College of Public Health, Hebei University, Baoding, 071002, China. Electronic address:

The illegal addition and abuse of 17β-estradiol (E2) in food has led to its accumulation in the body through the food chain, resulting in adverse effects on the human body through interference with the endocrine system. Because milk and dairy products are major components of the human diet, screening as well as quantitative analysis of E2 in these food types is important. In this work, a three-dimensional graphene/multi-walled carbon nanotube composite was synthesized and applied to a home-made pipette-tip solid-phase extraction cartridge and coupled with high-performance liquid chromatography-fluorescence detection to determine E2 in milk. The established method showed good linearity in the range of 5-250 ng mL with correlation coefficient of 0.9998. The detection limit and quantitation limit were 0.7 and 2.3 ng mL, respectively. The repeatability and intermediate precision, expressed as the coefficient of variation were 3.7% and 6.0%, respectively. The accuracy of the method was investigated by recovery experiments with milk at three spiked levels (25, 100, and 250 ng mL), where the recoveries were in the 88.4-108.9% range with relative standard deviations ≤5.5%. The proposed method has the advantage of requiring less adsorbent (only 1.0 mg) and less organic reagent (1.0 mL of washing solvent, 1.2 mL of elution solvent) and exhibits excellent purification ability, with high sensitivity and accuracy, and was successfully applied for the determination of E2 in milk products.
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http://dx.doi.org/10.1016/j.chroma.2019.04.055DOI Listing
August 2019

Green protocol for the preparation of hydrophilic molecularly imprinted resin in water for the efficient selective extraction and determination of plant hormones from bean sprouts.

Anal Chim Acta 2019 Aug 15;1064:47-55. Epub 2019 Mar 15.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, College of Public Health, Hebei University, Baoding, 071002, China; Key Laboratory of Analytical Science and Technology of Hebei Province & College of Chemistry and Environmental Science, Hebei University, Baoding, 071002, China. Electronic address:

In this study, a novel and green synthesis of a new hydrophilic molecularly imprinted 3-aminophenol-hexamethylenetetramine (MIAPH) resin for the selective recognition and separation of plant hormones was developed. The MIAPH resin was obtained using 3-aminophenol as multifunctional monomer which introduced hydroxyl, amino, and imino groups simultaneously, and adenine was used as a dummy template for molecular imprinting. Meanwhile, hexamethylenetetramine released formaldehyde slowly through hydrolysis which was used as the cross-linking agent to avoid the direct and excessive use of toxic formaldehyde. The entire procedure was performed under mild conditions, and was facile, environmentally friendly and energy-efficient. The obtained MIAPH resin showed high specific recognition toward plant hormones and higher recoveries in bean sprouts compared to NIAPH, HLB, and C. Various parameters affecting the extraction efficiency were optimized, and the calibration linearity of the MIAPH‒SPE‒HPLC method was determined from 0.07 to 2.86 mg kg with a correlation coefficient (r) ≥ 0.9994 under the optimal conditions. Recoveries of spiked standards ranged from 90.2 to 99.1% for bean sprout with a relative standard deviation of ≤5.3%. Finally, the established MIAPH‒SPE‒HPLC method was successfully applied for the selective extraction and sensitive detection of plant hormones in a variety of complex vegetable matrices.
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http://dx.doi.org/10.1016/j.aca.2019.03.025DOI Listing
August 2019

3-Aminophenol-glyoxylic acid resin for the determination of triazine herbicides in tomatoes.

Anal Chim Acta 2019 Jul 10;1061:122-133. Epub 2019 Feb 10.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education & College of Public Health, Hebei University, Baoding, 071002, China; Key Laboratory of Analytical Science and Technology of Hebei Province, College of Chemistry and Environmental Science, Hebei University, Baoding, 071002, China. Electronic address:

A facile and efficient method for the determination of triazine herbicides in tomato samples was developed by employing 3-aminophenol-glyoxylic acid resin microspheres as a solid-phase extraction adsorbent followed by high performance liquid chromatography analysis. These resin microspheres were synthesized by a simple green precipitation polymerization method, and a range of functional groups (hydroxyl, amino, carboxylic group) were introduced through the 3-aminophenol and glyoxylic acid components. The as-prepared resin microspheres were characterized by scanning electron microscopy, Fourier transform infrared spectrometry, and thermal gravimetric analyzer. The resin microspheres exhibited a good adsorption rate, large adsorption amount, and short adsorption equilibrium time (almost in ∼5 min). Under the optimal extraction and determination conditions, a good linearity was obtained in the range of 0.025-7.5 μg g (r ≥ 0.9997) for atraton, ametryn, and prometryn. The limits of detection of atraton, ametryn, and prometryn were 0.57, 0.75, and 1.06 μg kg, respectively. The intra-day and inter-day precisions expressed as relative standard deviations were in the ranges of 1.8-3.2% and 1.7-4.1%, respectively. In addition, the recoveries at three spiked levels ranged from 85.1 to 97.7% with the relative standard deviation ≤ 5.4% (n = 3). This novel method is simple and accurate and has proved to be a reliable alternative method for the determination of triazine herbicides in tomato samples.
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http://dx.doi.org/10.1016/j.aca.2019.01.062DOI Listing
July 2019

Fabrication of a monolithic, macroporous diallyl maleate-based material and its application for fast separation of intact proteins from human plasma with reversed-phase chromatography.

J Chromatogr A 2019 May 11;1592:197-201. Epub 2019 Jan 11.

Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, Hebei University, Baoding, 071002, China.

A monolithic diallyl maleate-based column was developed and used to separate intact proteins from complex bio-samples with high-performance liquid chromatography. The resulting monolith exhibited a relatively uniform porous structure with macro-pores. A sample of standard proteins mixture was used to explore the reversed-phase mechanism for fast separation on the homemade monolithic column. The observed retention time increased with the values of the diameters, relative hydrophobicities and molecular weights of the standard proteins, which mainly depends on the relative hydrophobicity of the proteins. It is worth mentioning that the mask of the three most abundant proteins in human plasma can be avoided, thus providing an opportunity for the middle- and low-abundance proteins to be detected. According to this exploration, the fast separation of human plasma proteins on the diallyl maleate-based monolithic column was achieved in 15 min. The chromatographic fractions were identified by liquid chromatography-tandem mass spectrometry, and the results indicate that the present method is an outstanding method for the fast and efficient fractionation of human plasma that will be significant sense for plasma proteomics research, especially for exploring new disease marker and drug target.
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http://dx.doi.org/10.1016/j.chroma.2019.01.026DOI Listing
May 2019

In situ synthesis of a monolithic material with multi-sized pores and its chromatographic properties for the separation of intact proteins from human plasma.

Talanta 2019 Mar 18;194:406-414. Epub 2018 Oct 18.

College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China.

The fabrication of a monolithic allyl phenoxyacetate-based material was proposed via the in situ radical polymerization using ethylene dimethacrylate as the crosslinker and 2,2'-azobisisobutyronitrile as the initiator within a stainless steel column (50 mm × 4.6 mm i.d.). The effects of the porogen composition, the crosslinker amount and the monomer type on the resulting monoliths were investigated. The morphology of the monoliths was characterized using scanning electron microscopy and a nitrogen adsorption-desorption instrument, and the pore structure was characterized using mercury intrusion porosimetry. The results indicate that the optimized monolith has a micro-, meso- and macro- multi-sized pore structure with a high specific surface area of 260.66 m g. The resulting monoliths were used as stationary phases for the separation of proteins from bio-samples, including a mixture of six standard proteins, chicken egg whites, snailase and human plasma, using high-performance liquid chromatography. Compared to optimized glycidyl methacrylate-based and styrene-based monolithic columns, the allyl phenoxyacetate-based monolithic column exhibited improved selectivity in the separation of proteins. Furthermore, the present method avoids the masking of highly abundant proteins, such as human serum albumin, immunoglobulin G and human fibrinogen, in the detection of middle- or low-abundance proteins in human plasma. The protein identification results obtained from liquid chromatography/mass spectrometry indicate that the present method is an outstanding method for efficient fractionation of human plasma, which will be especially useful in future plasma proteomics research.
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http://dx.doi.org/10.1016/j.talanta.2018.10.054DOI Listing
March 2019

A novel poly (NMA-co-DEA-co-EDMA) monolithic column as a sorbent for online solid-phase extraction and its application in the determination of β-sitosterol in plant oil samples.

Food Chem 2019 Apr 22;278:594-600. Epub 2018 Nov 22.

Key Laboratory of Pharmaceutical Quality Control of Hebei Province, College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China; Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, Baoding 071002, China. Electronic address:

A novel monolithic column was prepared by in-situ free radical polymerization using N-methylolacrylamide (NMA) and N,N-diethylacrylamide (DEA) as co-monomers. The monolith was characterized by scanning electron microscopy (SEM) and its nitrogen adsorption-desorption isotherm, and it was used as a solid phase extraction (SPE) absorbent for the online enrichment of β-sitosterol by high performance liquid chromatography. The optimized method had good linearity, and the linear regression coefficient was 0.998. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.006 mg/mL and 0.02 mg/mL, respectively. The interday and intraday accuracies were less than 7.28%. The spiked recoveries of β-sitosterol in the six plant oil were 90.96-103.56%. The maximum amount of β-sitosterol adsorbed on the monolithic column was 12.69 mg/g, and the enrichment factor of β-sitosterol was 78. The results showed that the monolith could be used as an online SPE absorbent for the determination of β-sitosterol in plant oil samples.
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http://dx.doi.org/10.1016/j.foodchem.2018.11.104DOI Listing
April 2019