RSC Advances
·
2021
·Vol. 11
·期 63
·39821-39828
·
IF 3.361
Baoyue Zhang,Yukui Tong,Jianghua He,Baodong Sun,Feng Zhang,Miaomiao Tian
Luteolin (LTL) is a flavonoid containing a cis-diol, which has significant anti-inflammatory, anti-allergic, anti-diabetic, anti-cancer and neuroprotective activities. In this work, a silver modified boric acid affinity polyvinyl imine (PEI) dendritic adsorbent (PPEI-Ag@CPBA) was prepared on polystyrene (PS) for the rapid recognition and selective separation of LTL. A thin layer of polydopamine (PDA) was formed on the surface of the substrate by self-polymerization, and a PDA-coated PS material (PS@PDA) was obtained. PEI with sufficient active amino groups was grafted onto PS@PDA to obtain a PEI-modified material (PS@PDA@PEI), then AgNO3 was reduced with NaBH4, and PS@PDA@PEI was embedded on Ag. Finally, PPEI-Ag@CPBA was obtained through the condensation reaction of PEI with 4-carboxyphenyl boric acid (CPBA). The adsorption conditions were optimized, the optimal pH and the optimum amount of adsorbent were determined, and the maximum adsorption capacity was found to be 2.49 mg g−1. This method has been successfully applied to the selective identification of LTL in peanut shell samples, and provides a practical platform for the detection of LTL in complex substrates.
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FOOD CHEMISTRY
·
2021
·
IF 7.514
Liye Wang,Jiangxiu Niu,Pengyuan Wei,Yilei Feng,Mingyue Ding,Chaojun He,Yongjie Ma,Yaolei Zhu,Jia Li,Lingli Huang,Xiya Zhang
To reduce matrix interference and realize simultaneous detection of multiple homologous compounds (trimethoprim (TMP), diaveridine (DVD), ormetoprim (OMP), baquiloprim (BQP), and aditoprim (ADP) in pig, cattle, chicken, and fish muscles), an immunomagnetic bead (IMB)-based sample purification pretreatment with HPLC–UV was developed. A broad-spectrum monoclonal antibody (mAb, named 14C6) was prepared and conjugated with carboxylic-acid-functionalized magnetic nanoparticles using the active ester method to obtain IMBs for sample purification. The extraction solvent was optimized based on the extraction efficiency. Good linearity was observed for all the five analytes (10–200 μg/kg) with the LOD and LOQ of 5 and 10 μg/kg, respectively. The mean recoveries ranged from 62.5% to 76.9%, while the coefficient of variation was <12.2%. The IMB method afforded greater sample purification and enrichment than those achieved with the SPE column-based conventional method. Hence, the IMB-based sample purification is a useful tool to determine 2,4-diaminopyrimidine residues in edible animal tissues.
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JOURNAL OF MOLECULAR STRUCTURE
·
2022
·
IF 3.841
Wan-ping Chen,Run-quan Wang,Yue-rong Zhang,Kai Song,Yuan Tian,Jia-xian Li,Guo-ying Wang,Gao-feng Shi
In this article, the scavenging ability of hypericin on hydroxyl radicals was evaluated by UV spectra, HPLC and fluorescence spectra. The reaction mechanism of the scavenging of free radicals by hypericin was also investigated. The Gaussian calculations obtained for the spatial structure and electrostatic potential of hypericin revealed that the active site for the reaction of hypericin with hydroxyl radicals is on the phenolic hydroxyl group of hypericin. The dissociation energy, spin density and frontline orbitals of the dehydrogenated hypericin radicals yielded that hypericin 7-OH and 7′ -OH are most likely to react with hydroxyl radicals. the transition state structure, enthalpy change and Gibbs free energy change and energy change of the reaction between hypericin and hydroxyl radicals,and the results of the above calculations indicate that hypericin 7-OH and 7′ -OH have the highest activity, can be directly involved in the scavenging process of radicals, followed by 5-OH and 5′ -OH, and finally 4-OH (4′ - OH).In-depth study of the antioxidant mechanism of hypericin molecules can help to design and synthesize new antioxidants in a more rational way.
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FOOD CHEMISTRY
·
2020
·
IF 6.306
Tian-Qin Peng,Xiao-Li Yin,Hui-Wen Gu,Weiqing Sun,Baomiao Ding,Xian-Chun Hu,Li-An Ma,Shu-Dong Wei,Zhi Liu,Shi-Yi Ye
Laoshan green teas plucked in summer and autumn were measured by high performance liquid chromatography-diode array detector (HPLC-DAD). After baseline correction, the fingerprints data were resolved by multivariate curve resolution-alternating least squares (MCR-ALS) and a total of 57 components were acquired. Relative concentrations of these components were afterwards applied to distinguish plucking seasons using principal component analysis (PCA), support vector machines (SVM) and partial least squares-discriminant analysis (PLS-DA). For both SVM and PLS-DA models, the total recognition rates of training set, cross-validation and testing set were 100%, 91.3% and 100%, respectively. Besides, three variable selection methods were employed to determine characteristic components for the authentication of summer and autumn teas. Results showed that PLS-DA model based on three characteristic components selected by VIP possesses identical predictive ability as the original model. This study demonstrated that our proposed strategy is competent for the authentication of plucking seasons of Laoshan green tea.
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BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 34
·期 9
·e4901
·
IF 1.728
Guangjiao You,Chenghao Li,Yingying Mao,Xiaoliang Ren,Yanan Liu,Meng Wang
Radix Paeoniae Alba (RPA) and its processed products are commonly used in traditional Chinese medicine, but the chaos phenomenon among processed products often occurs. In this study, we used multiple chemometric methods to analyze raw and six different processed products of RPA based on HPLC fingerprinting. Heat map analysis was used to assess the changes in chemical composition. Principal component analysis was used for classification, and the samples were divided into four classes: class 1 (raw, wine-processed, and vinegar-processed products), class 2 (bran-processed and soil-processed products), class 3 (stir-fried products), and class 4 (coke products). Further, the orthogonal partial least squares discriminant analysis model was used to obtain chemical markers among different classes. The antioxidant property of RPA is an important factor responsible for its pharmacological effects, and so the antioxidant activity of RPA was also investigated. We measured 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) and hydroxyl radical scavenging ability, and ferric reducing antioxidant power. The total antioxidant activity follows the order: coke > stir-fried > soil-processed > bran-processed > wine-processed > raw > vinegar-processed products. These results suggest that different processing methods affect the chemical composition and antioxidant power of RPA, and thus, different products of RPA should not be mixed.
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MICROCHEMICAL JOURNAL
·
2019
·
IF 3.206
Hui Guo,Yunfei Chen,Na Song,Xinyi Yang,Shen Yao,Junqing Qian
Bamboo leaf is known as dietic tea for the prevention of obesity in China. To screen lipase inhibitors from bamboo leaf extract rapidly, lipase functionalized magnetic ligand fishing combined with HPLC/MS was established. Firstly, lipase was immobilized on magnetic nanoparticles by dialdehyde starch to obtain lipase-functionalized magnetic nanoparticles (L-MNPs), and then the L-MNPs were incubated with bamboo leaf extract to fish out ligands. Three enzyme inhibitors were obtained and identified as isoorientin, orientin, isovitexin by HPLC/MS. The results provided a powerful evidence for explaining the hypolipidemic effects of bamboo leaf extract, and this ligand fishing method is feasible for screening enzyme inhibitors from complex mixtures.
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Analytical Methods
·
2019
·Vol. 12
·期 2
·141-148
·
IF 2.378
Xue Ren,Man He,Beibei Chen,Bin Hu
Herein, magnetic porous organic polymers (MOPs) prepared via an azo coupling reaction in water under mild conditions are evaluated for the extraction of seven cardiovascular drugs, including xylocaine, metoprolol, mexiletine, labetalol, propranolol, carvedilol and propafenone, from human urine samples for the first time. The extraction mechanisms are assumed to be electrostatic interaction and π–π stacking. The MOPs exhibited fast adsorption/desorption time (13 min) and high enrichment factors (315–365-fold) for target analytes. Based on this, a method coupling magnetic solid phase extraction with HPLC-UV detection was developed for the analysis of cardiovascular drugs. Under the optimized conditions, the LODs (S/N = 3) were in the range of 0.06–0.57 μg L−1 with an RSD (n = 5) of 4.3–8.6%, and the linear range was 0.2–200 μg L−1 for propranolol, 2–200 μg L−1 for metoprolol, and 0.5–200 μg L−1 for the other five analytes. The developed method was applied for the analysis of cardiovascular drugs in urine samples with recoveries of 89.0–112%. In order to further evaluate the application potential of this method, real-time monitoring of metoprolol in urine samples collected from volunteers treated with metoprolol tablets was performed. The proposed method is simple, fast, and sensitive and has good potential in the monitoring of cardiovascular drugs in competitive sports and clinical analysis.
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JOURNAL OF AOAC INTERNATIONAL
·
2019
·Vol. 98
·期 2
·422-430
·
IF 1.201
Zong Yingying,Lin Jia,Xu Hua,Jia Zhihui,Yang Xiupei,Choi Martin M F
A novel isocratic RP–HPLC method with UV photodiode array detection for the determination of seven organic acids in vinegar samples was developed and optimized. Samples were analyzed on a C18 (150 × 4.6 mm id, 5 μm) analytical column. Methanol–0.010 M sodium dihydrogen phosphate buffer adjusted with H3PO4 to pH 2.80 (2 + 98, v/v), was used as the mobile phase. The column oven temperature was optimized at 23.0°C, the flow rate was 0.80 mL/min, and the detection wavelength was 210 nm. Matrix-matched calibration curves were prepared for all analytes, and the correlation coefficients were greater than 0.99. LOD and LOQ ranged from 0.10 to 10.0 and 0.30 to 30.0 μg/mL, respectively. The results for interday and intraday precision and accuracy fell within the ranges specified. Vinegar samples were quantified by the standard addition method. The main advantages of this method are its selectivity, which is one of themain weaknesses of most methods when determining organic acids in complex matrixes, and its simplicity since little sample preparation is needed. Moreover,it is safe and inexpensive with low organic solvent usage.
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RSC Advances
·
2019
·Vol. 9
·期 44
·25797-25804
·
IF 3.049
Shunli Ji,Hongbin Gao,Xingya Xia,Feng Zheng
Benzyl halides, widely used as alkylation reagents in drug synthesis, are potential genotoxic impurities (PGTIs) required to be controlled at trace levels. However, the existing analytical methods for benzyl halides often suffer from matrix interferences or low derivatization efficiency of benzyl chlorides. In this paper, a simple derivatization HPLC-UV method was developed for the analysis of these residual trace benzyl halides in drug substances. 1-(4-Nitrophenyl) piperazine (4-NPP) was selected as a new derivatization reagent because it shifted well the benzyl halides derivatives away to the near visible range (392 nm), which could minimize the matrix interferences from the drug substances and related impurities. Meanwhile, potassium iodide (KI) was used to convert the mixed benzyl halides into benzyl iodides before derivatization. The derivatization parameters were also optimized using the design of experiments (DoE) for achieving the best reaction efficiency. The results showed that the new approach had high specificity and sensitivity, and the LOQs were 7–9 μg g−1 relative to 5 mg mL−1 antipyrine and 17.5–22.5 μg g−1 relative to 2 mg mL−1 oroxylin A. The method is a valuable alternative for the determination of residual benzyl halides in the drug substances.
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MICROCHIMICA ACTA
·
2018
·Vol. 185
·期 7
·1-8
·
IF 5.705
Wei Lanlan,Song Yuan,Liu Ping,Kang Xuejun
Polystyrene nanofibers were coated with copper nanoparticles (CuNPs) by a combination of electrospinning and in-situ reduction of Cu(II) using sodium borohydride as the reductant. The CuNPs on the nanofibers were characterized by energy dispersive spectrometry, scanning electron microscopy and transmission electron microscopy. A cartridge was packed with the nanofibers which then were activated with methanol and water. Glutathione (GSH) is found to quantitatively adsorbed by the packed cartridge at pH 3.0, and then can be desorbed with aqueous 2-mercaptoethanol and detected, after derivatization with ortho-phthalaldehyde, via high performance liquid chromatography with fluorometric detection. Under optimized conditions, the method has a 1.1 ng·mL −1 detection limit and a response that is linear in the 10–1000 ng·mL −1 GSH concentration range. The recoveries of GSH from artificial urine spiked at three levels (80, 400 and 800 ng·mL −1 ) are in the range of 94.6–98.6% with relative standard deviations (RSD) of <4.5% ( n = 5). The method was applied to assessing the differences in urinary GSH between high-risk infants and healthy infants. The results show that the levels of GSH of normal infants are significantly higher than those of high-risk infants ( P < 0.05).
Schematic of the preparation of CuNP-assembled nanofibers and the mechanism of extracting glutathione (GSH). GSH can be extracted by this material based on a strong interaction between the sorbent and GSH. This is attributed to the formation of Cu-S bonds between Cu and -SH.
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Analytical Methods
·
2018
·Vol. 10
·期 41
·4978-4984
·
IF 2.073
Xing Huang,Kaipeng Zhang,Yanli Tong,Yongsheng Zhong,Zuanguang Chen
In this study, a gradient reverse phase high performance liquid chromatography combined with a capacitively coupled contactless conductivity detection (RP-HPLC-C4D) method for simultaneous determination of phospholipid and fatty glyceride in liposome was developed. After saponification, the fatty glyceride and two types of phospholipids were transformed into octanoic acid, palmitic acid and erucic acid, respectively, which were then separated and detected by RP-HPLC-C4D. The results showed good linearity in the range of 20–1000 μg mL−1 for octanoic acid and erucic acid and 10–1000 μg mL−1 for palmitic acid. The LODs of octanoic acid and palmitic acid reached 2.5 μg mL−1, and 10 μg mL−1 for erucic acid. The average recoveries of octanoic acid, palmitic acid and erucic acid were 100.2%, 102.9% and 101.4% (n = 9), respectively. The developed method could be effectively applied in the quality control and stability monitoring of liposome.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2018
·Vol. 411
·期 2
·507-515
·
IF 3.307
Yang Yi,Yin Shuo,Yang Danni,Jiang Yang,Li Yongxin,Zhou Chen,Sun Chengjun
A novel carboxyl Fe 3 O 4 magnetic nanoparticle-based solid-phase extraction combined with high-performance liquid chromatography was developed for the analysis of oxytetracycline, tetracycline, demeclocycline, metacycline, chlortetracycline, and doxycycline in water samples. Driven by the electrostatic interaction and the strong chelation between tetracyclines and iron ions, tetracyclines in samples were adsorbed onto the adsorbents. The adsorbed analytes were subsequently eluted with oxalic acid and separated with a C 18 column under gradient condition with a mobile phase consisting of methanol, acetonitrile, and oxalic acid at a flow rate of 0.5 mL/min. The detection was performed at variable ultraviolet wavelengths. Under optimized conditions, the developed method gave an enrichment factor of 33.3, linearity ranges of 5.00–1000 μg/L, detection limits of (2.86–5.19) × 10 -2 μg/L, quantification limits of (9.54–17.3) × 10 -2 μg/L, recoveries of 76.2–98.0%, and intra- and inter-day RSDs of 0.132–15.5% and 2.28–14.5% for these tetracyclines. The established method was successfully applied for the determination of these six tetracyclines in tap water, river water, pond water, and lake water samples.
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