JOURNAL OF FOOD AND DRUG ANALYSIS
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2020
·
IF 4.727
Li Li,Meng-Lin Fan,Ya-Nan Li,Ya-Xuan Huang,Xiu-Feng Liu,Ji-Hua Liu
Proprotein convertase subtilisin/kexin type 9 (PCSK9) is an attractive target for new cholesterol-lowering drug development. Here, we developed a method integrating ligand fishing, HPLC-Q-TOF-MS and interdisciplinary assay, aiming to explore potential PCSK9 inhibitors from mixtures rapidly and accurately. PCSK9 was expressed and purified firstly, and then the recombined PCSK9 was coated on the surface of magnetic beads (MBs). The PCSK9-immobilized MBs (PCSK9-MBs) were used for ligand fishing combined with HPLC and Q-TOF-MS/MS. Ginkgo biloba leaves (GBL), an herbal medicine widely used in Asia and Europe with good efficacy in treatment of hypercholesterolemia, were chosen as an illustration for ligand fishing. Two PCSK9 ligands were discovered from GBL and identified as kaempferol-3-O-rutinoside (1) and kaempferol 3-O-26″-(6‴-p-coumaroyl) glucosylrhamnoside (KCGR) (2). In order to verify fishing results and pick out more powerful PCSK9 inhibitors, molecular docking assay was further performed and KCGR was optimized to be an excellent PCSK9 inhibitor by the confirmation of affinity and activity bioassay. These results suggested that the developed approach could be applied to screen and analysis potential bioactive constituents from mixtures, which may improve the efficiency of drug discovery. Moreover, KCGR separated from GBL was expected to be a potential candidate of PCSK9 inhibitors.
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FOOD CHEMISTRY
·
2019
·
IF 5.399
Yun-Jiao Ma,An-Qi Bi,Xiao-Yuan Wang,Lei Qin,Ming Du,Liang Dong,Xian-Bing Xu
The dispersion solid-phase microextraction (DSPE) combined with dispersion liquid–liquid microextraction (DLLME) was developed as a rapid, simple and effective pretreatment method for the determination of flavor enhancers (maltol, ethyl maltol, vanillin, methyl vanillin, ethyl vanillin) of ready-to-eat seafood products (dried squid, baked squid, fried fish, steamed abalone). Under the optimized DSPE–DLLME method, the developed method exhibited low limits of quantitation (0.20–0.50 μg g −1 ) and excellent linearity (R 2 ≥ 0.995). The recoveries of flavor enhancers in the actual samples were 83.7%–114.9%. Compared with traditional pretreatment methods, the developed DSPE–DLLME method was rapid (17 min) and easy to determine the flavor enhancers by high performance liquid chromatography with photodiode array detector (HPLC-PDA). In the actual samples, creamy compounds such as vanillin, methyl vanillin and ethyl vanillin were hardly found. However, the flavor compounds produced by thermal reactions such as maltol (except for dried squid 3) and ethyl maltol were present in all samples.
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INDUSTRIAL CROPS AND PRODUCTS
·
2019
·
IF 4.191
Xiaoqi Chen,Wei Wang,Cheng Wang,Zijia Liu,Qi Sun,Dongmei Wang
Zanthoxylum bungeanum leaves (ZBL) have rich flavonoids with a variety of bioactivities, which has great values of development and utilization. In this paper, the quality of thirteen varieties of ZBL collected from a common garden was evaluated based on flavonoids compositions, bioactivity and reversed-phase high performance liquid chromatography (RP-HPLC) fingerprint coupled with chemometrics analysis. The values revealed that You Huajiao (S13) exhibited the highest contents of flavonoids compounds and strongest bioactivity, followed by Hancheng Dangcun stingless (S1). Among different varieties HPLC-fingerprint, eight common characteristic peaks were selected and the similarity lay within the range of 0.502-0.999. Meanwhile, thirteen varieties were divided into four groups (G1-G4) and two discriminant functions with the discriminant rate of 100% were constructed. Additionally, quercitrin and afzelin were found to be key compounds of quality evaluation. In conclusion, G4 (You Huajiao, S13) was selected as the best variety, followed by G1 (S1, S3, S5, S6, S7, S10, S12) and G2 (S4, S8, S9, S11), respectively, and G3 (Fugu late-maturing, S2) was at the last level. Consequently, this study screened for fine varieties of ZBL and provided a basis for the development and utilization of high-quality resources of Z. bungeanum .
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2019
·
IF 2.813
Xi Zhou,Huiqin Wu,Xiaolan Huang,Fang Hang,Huitai Luo
This study established a simple and rapid method for simultaneous determination of short-chain chlorinated paraffins (SCCPs) and medium-chain chlorinated paraffins (MCCPs) in human serum by high performance liquid chromatography coupled with electron spray ionization quadrupole time-of-flight mass spectrometry (HPLC-ESI-Q-TOF/MS). A simple pretreatment procedure of protein precipitation by acetonitrile coupled with liquid-liquid extraction by n-hexane was employed for extraction and purification . The purified samples were separated by a PFP chromatographic column. This method could effectively eliminate the matrix effect by lipids and other matrix substances in serum samples with less time and solvent consuming. 76 congener groups of SCCPs and MCCPs with C 10 -C 17 and Cl 5 -Cl 13 were quantified by their [M-H] − ions. Method detection limit (MDL) were 1.0–8.0 ng mL −1 for ∑SCCPs and ∑MCCPs. Recoveries were 98.4 ± 4.42%, 98.8 ± 3.96% and 90.7 ± 2.79% for SCCPs and 93.1 ± 6.67%, 108 ± 1.21% and 90.8 ± 3.78% for MCCPs at spiking concentrations of 20, 50 and 200 ng·mL −1 , respectively. The relative standard deviations (RSDs) of intra- and inter-day variations were 1.41% and 9.84% for SCCPs, and 4.23% and 6.26% for MCCPs. The suitability of the developed method was demonstrated through the application to analysis of SCCPs and MCCPs in human serum samples.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Bolin Zhu,Mengyao Xue,Beibei Liu,Qing Li,Xingjie Guo
In the present paper, a sensitive and selective chiral LC method has been developed for enantiomeric separation and determination of eight antihistamines in pharmaceutical formulations. Enantiomeric separation was achieved on the α 1 -acid glycoprotein-based chiral stationary phase known as Chiralpak AGP. The effects of the mobile phase composition, type and proportion of organic modifier and the concentration and pH of the buffer on retention and resolution were fully investigated. All enantiomers of target analytes were successfully separated with the mobile phase consisting of methanol and 10 mM ammonium acetate buffer, at a flow rate of 0.9 mL min −1 . Calibration curve of each enantiomer was linear over the concentration range of 5.0–100 μg mL −1 , with the correlation coefficient above 0.9990. The limits of detection and quantification were below 0.80 and 3.18 μg mL −1 , respectively. The recoveries were in the range of 98.0–102.4% with the relative standard deviation lower than 2.88% for all enantiomers. The validated method was demonstrated to be suitable for the quality control of the enantiomeric composition of antihistamines present in pharmaceuticals. Finally, the proposed chiral LC method was applied to the determination of antihistamines enantiomers in commercially available tablets containing racemic mixtures of compounds. Quantitative results of the commercial tablets demonstrated that the difference between the declared and determined values did not exceed 1.45%, and chiral antihistamines drugs were present in the form of racemates.
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CHROMATOGRAPHIA
·
2019
·Vol. 83
·期 2
·173-181
·
IF 1.552
Li Mingxue,Bai Ligai,Sun Fanrong,Peng Shan,Liu Haiyan,Ma Zhengyue
Abstract A four-hydrogen furfuryl-based polymer monolithic column for solid-phase extraction was prepared via in situ radical polymerization, using tetrahydrofurfuryl methacrylate as the monomer. The monolith was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy and nitrogen adsorption–desorption method, showing relatively uniform porous structure with micro-, meso- and macro-pores and a relatively high surface area of 54.99 m 2 g −1 . Online solid-phase extraction–high-performance liquid chromatography was carried out to quantitatively analyze six alkaloids, including caffeine, hydroxy-α-sanshool, hydroxy-β-sanshool, hydroxy-γ-sanshool, hydroxy-γ-isosanshool and γ-sanshool in rat plasma. The results show that the prepared polymer monolithic sorbent exhibits good clean-up ability for bio-matrix, as well as good extractive ability for the six concerning alkaloids in rat plasma. Method validation shows that the correlation coefficients of the linear regressions are higher than 0.998 and the accuracy represented by spiked recovery ranges in 94.37–100.7%, 99.52–101.1%, 98.93–100.8%, 98.36–101.6%, 99.22–101.2% and 99.86–101.4% for the six alkaloids, respectively, as well as the LOD ranges in 2.10–3.90 ng mL −1 and the LOQ in 6.35–10.14 ng mL −1 . Compared to the reference works, the present work is a simple and effective method for online extraction and simultaneous determination of six alkaloids in plasma with high accuracy and low cost. Graphic Abstract
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Food Analytical Methods
·
2018
·Vol. 11
·期 10
·2885-2896
·
IF 2.245
Qi Mengyu,Tu Chunyan,Li Zhaoqian,Wang Weiping,Chen Jianrong,Wang Ai-Jun
A rapid, sensitive, and economical pipette tip solid phase extraction (PT-SPE) based on graphene oxide/polypyrrole (GO/PPy) coupled with high performance liquid chromatography (HPLC) was developed for the extraction and determination of sulfonamides (SAs) in honey and milk samples. The PT-SPE procedure involved only 3.0 mg of adsorbent, 3 min adsorptive extraction time, and less than 1.0 mL of solvent consumption (sample, washing, or eluent). Under the optimal conditions, good linearities (0.01–10.00 μg mL −1 ) were obtained with correlation coefficients ( r ) > 0.9996. The limits of detection ( S / N = 3) were in the range of 1.04–1.50 ng mL −1 . Meanwhile, the proposed method was successfully applied for the analysis of SAs in honey and milk with average recoveries within 62.3–109.0% and relative standard deviations less than 11.2%. The results demonstrated that the developed PT-SPE-HPLC method was suitable for the analysis of SAs in complex matrix due to its high sensitivity and accuracy.
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TALANTA
·
2015
·
IF 3.545
Qiyuan Shi,Jiale Chen,Qinfen Zhou,Houliang Lei,Lianjun Luan,Xuesong Liu,Yongjiang Wu
A rapid and efficient method for the identification of antioxidants in the traditional Chinese medicine Polygalae Radix (PR) by HPLC–ESI-Q-TOF-MS/MS is described. The method is based on the hypothesis that upon reaction of antioxidants with 1,1-diphenyl-2-picrylhydrazyl (DPPH), the peak areas of compounds with potential antioxidant activities in the HPLC chromatogram will be significantly reduced in comparison to the untreated sample. The identity confirmation was achieved by Q-TOF-MS/MS technique. With this method, eight components were proposed possessing potent antioxidant activity. They were identified as sibiricose A5, sibiricose A6, sucrose monoester, polygalaxanthone III, tenuifoliside B, 3',6-disinapoylsucrose (DISS), sucrose diester , tenuifoliside C, respectively. DISS was proposed to be the most potent one. The antioxidant activity of DISS was evaluated by DPPH, ABTS radical scavenging assay and ferric-reducing antioxidant power (FRAP) assay in vitro. Vitamin C (Vc) was used as positive control substance. DISS showed moderate DPPH (DISS's IC 50 value was 1024.17 μg/mL, Vc's was 294.68 μg/mL) and ABTS (IC 50 324.13 μg/mL, Vc's was 117.50 μg/mL) free radical scavenging capacity and ferric-reducing antioxidant power. DISS can be used as a new source of natural antioxidant in foods and cosmetics.
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Food Analytical Methods
·
2013
·Vol. 7
·期 7
·1381-1386
·
IF 1.969
Ma Xiaoxing,Wang Juntao,Wu Qiuhua,Wang Chun,Wang Zhi
A new analytical method by graphene-reinforced hollow fiber liquid-phase microextraction combined with high-performance liquid chromatography fluorescence detection was developed for the determination of bisphenol A and 4- tert -butylphenol in bottled juices. Several important experimental parameters were studied to get optimal extraction conditions for the analytes. Under the optimized conditions, the method showed a good performance having a linear response in the range from 0.05 to 10.0 ng mL −1 with the correlation coefficients ( r ) of 0.9965–0.9994 and limits of detection of 0.01 ng mL −1 . The relative standard deviations were in the range from 6.4 to 7.2 % at the spiked concentration of 1.0 ng mL −1 . The method combines the high-adsorption capacity of graphene and the excellent clean-up performance of hollow fiber liquid-phase microextraction and has been successfully applied to the analysis of the analytes in bottled juice samples.
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Analytical Methods
·
2015
·Vol. 8
·期 5
·1003-1012
·
IF 1.821
Xiaoxiao You,Ligang Chen
A new strategy for the isolation and enrichment of sulfonylurea herbicides in grain samples was obtained by using magnetic molecularly imprinted polymers (MMIPs) using carbon nanotubes as the matrix, nicosulfuron as the template molecule, 3-aminopropyltriethoxysilane as the functional monomer, tetraethyl orthosilicate as the cross-linker and cetyl trimethylammonium bromide as the dispersant. The characteristics of the MMIPs were assessed by transmission electron microscopy, vibrating sample magnetometry, X-ray diffractometry, elemental analysis, the Brunauer–Emmett–Teller method and Fourier transform infrared spectroscopy. The binding characteristics of the imprinted materials were researched using isothermal adsorption experiments, kinetics adsorption experiments and selectivity experiments. The recoveries of four sulfonylurea herbicides were more than 80.0% and the detection limits were 0.0107, 0.0151, 0.0147 and 0.0123 μg g−1, respectively. RSDs of intra-day and inter-day precisions in the range of 0.7–2.4% and 5.3–8.4% were obtained, respectively. The results demonstrate that MMIPs are promising for the preconcentration, purification and analysis of sulfonylurea herbicides in grain samples.
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TALANTA
·
2014
·
IF 3.511
Minqiong Tang,Qing Wang,Ming Jiang,Li Xu,Zhi-Guo Shi,Ting Zhang,Yan Liu
In the present study, magnetic nanoparticles (MNPs) with phenyl functionalized core and a hydrophilic methylcellulose coating were synthesized. The functionalized MNPs showed excellent dispersibility in aqueous solution and they were applied to magnetic solid phase extraction (MSPE) of sildenafil and its metabolite, desmethyl sildenafil, from human urine and plasma samples followed by high performance liquid chromatographic analysis. The factors that may influence the extraction, including the amount of MNPs, pH and salt concentration of sample solution, extraction and desorption time, and the volume of desorption solvent, were investigated in detail. Under the optimum MSPE conditions, the developed method showed satisfactory reproducibility with intra-day and inter-day relative standard deviations less than 8.2% and low limits of detection of 0.41–0.96 ng mL −1 from urine and plasma samples. The proposed material possessed good water compatibility and demonstrated excellent applicability for biological samples.
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Food Analytical Methods
·
2014
·Vol. 8
·期 2
·428-437
·
IF 1.802
Zeng Fang,Ou Jun,Huang Yufen,Li Qian,Xu Guizhi,Liu Zhongzhen,Yang Shaohai
The present paper reports the application of an optimized pre-column derivatization procedure with aminoquinolyl- N -hydroxysuccinimidyl carbamate (AQC) to the determination of 21 free amino acids in fruit juices. The method permitted the optimal separation of 21 amino acids and ammonium in 30 min. Excellent response linearity was obtained from 2 to 1,000 μM for all amino acids, except tryptophan, for which the linearity was 5–1,000 μM. The fluorescence detection limits ranged from 0.08 pmol (phenylalanine) to 0.69 pmol (cysteine), except for tryptophan (7.89 pmol), for a signal-to-noise ratio of 3. The relative standard deviations of peak areas ranged from 0.1 to 0.4 % for intraday analysis and from 2.1 to 5.0 % for interday analysis. The method was applied to analyze the free amino acids in six fruit juices, and the recoveries of the proposed method were 90.4 to 103.3 %. The total free amino acid content ranged from 56.97 mg L −1 (apple) to 469.45 mg L −1 (longan) in six fruit juices. Aspartic acid (Asp), glutamic acid (Glu), asparagine (Asn), serine (Ser), and glutamine (Gln) were present in higher levels in most samples, whereas cysteine (Cys) was below the detection limit in the selected samples. Notable advantages of this method include its speed, ease, low cost, good repeatability, high sensitivity, excellent precision and accuracy, and anti-interference in high-sugar matrices.
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危险品化学品经营许可证（带存储）