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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2018 · IF 2.831

Simultaneous determination of tryptophan, kynurenine, kynurenic acid and two monoamines in rat plasma by HPLC-ECD/DAD

Ting-ting Du,Ting Cui,Hong-mei Qiu,Nian-ru Wang,Dan Huang,Xin-hui Jiang

A high-performance liquid chromatography method with a diode array and an electrochemical detection (HPLC-ECD/DAD) was developed to determine the levels of tryptophan (TRP), kynurenine (KYN), kynurenic acid (KYA), 5-hydroxytryptamine (5-HT) and 5-hydroxyindoleacetic acid (5-HIAA) in rat plasma. The prepared samples were separated on a BDS column (4.6 mm × 250 mm, 5 mm) with column oven temperature of 25 °C. The mobile phase consisted of 5% acetonitrile and a buffer solution, which contained 25 mmol/L sodium acetate and 0.01 mmol/L EDTA, adjusting pH to 4.5 with acetic acid, and it was pumped at a flow-rate of 1.0 mL/min. KYN and KYA were measured by a variable wavelength detector at wavelengths 360 nm and 333 nm respectively, TRP and vanillic acid (as IS) both were measured at 280 nm. Determination of 5-HT and 5-HIAA was accomplished at the electrochemical working potential of 700 mV. Total run time was 14 min. Several parameters of the developed method were validated including linearity, accuracy precision, and stability. The results showed the established method had good LOD and separation for all of the five compounds and IS in the biological matrix. The method is simple, fast, economical and accurate. The analytical method and the results could provide a reference for the clinical and scientific research of depression.

研究领域: 分析化学 · 神经科学 · 药理学
✓ 已验证 DOI 高影响因子
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JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES · 2018 · IF 0.827

Simultaneous quantification of urea and allantoin in cosmetic products by nano-HPLC using a highly hydrophilic monolith

Huihui Wu,Hanying Jin,Guangxin Yuan,Jacques Crommen,Jing Zhang,Qiqin Wang

Urea and allantoin are two important additives in cosmetic products for the treatment of dry skin as well as for skin protection and regeneration. In this research, a highly hydrophilic monolith prepared by co-polymerization of N,N-dimethyl-N-acryloyloxyethyl-N-(3-sulfopropyl)ammonium betaine (SPDA) and N,N’-methylenebisacrylamide (MBA) was first exploited for the simultaneous quantification of urea and allantoin in cosmetic products by nano-HPLC in the HILIC mode. The whole separation process could be completed within six minutes using isocratic elution. Due to the extremely high hydrophilicity of this monolithic column, a relatively low content (80%) of ACN in the mobile phase was required to achieve satisfactory separation, and therefore the solubility problems for polar compounds was also avoided in comparison with previously reported results on the commercial columns. Method validation was also accomplished with respect to linearity, reproducibility, selectivity, recovery, stability, LOD and LOQ. The recoveries of urea and allantoin from spiked cosmetic samples were 95.6%-100% and 94.1%-99.9%, respectively. Validation results indicate that this HILIC method based on the miniaturized poly(SPDA-co-MBA) monolith can be applied successfully to the fast and efficient determination of urea and allantoin in cosmetic samples. The miniaturized column format, the low sample consumption (20 nL), and excellent separation efficiency could make this highly hydrophilic monolith an attractive choice for the detection of trace polar analytes from complex samples in future.

研究领域: 分析化学 · 化妆品科学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2014 · IF 2.694

Rapid and sensitive HPLC–MS/MS method for quantitative determination of lycorine from the plasma of rats

Xin Liu,Yuan Hong,Qing He,Kai Huang

A simple, rapid and sensitive high-performance liquid chromatography–tandem mass spectrometric (HPLC–MS/MS) method was developed and validated for determining lycorine in rat plasma. Plasma samples were prepared by a simple protein precipitation with methanol containing dextrorphan as internal standard. The chromatographic separation was performed on a Kromasil 60-5CN column (3   μm, 2.1   mm   ×   150   mm) with the mobile phase of methanol/water (containing 0.1% formic acid) (40:60, v/v) at a flow rate of 0.2   mL/min, the total analytical runtime was 5   min. The detection was performed on a triple quadrupole tandem mass spectrometer equipped with Electronic Spray Ion by selected reaction monitoring (SRM) of the transitions at m / z 288.1   →   147.1 for lycorine and m / z 258.1   →   157.2 for dextrorphan, respectively. The calibration curve was linear over the range of 1–1000   ng/mL with the lower limit of quantification of 1   ng/mL for lycorine. The intra- and inter-day precision (R.S.D.%) were less than 8.5% and accuracy (R.E.%) was within ±7.0%. Lycorine was sufficiently stable under all relevant analytical conditions. This method was successfully applied to the pharmacokinetic study of lycorine in rats after intraperitoneal administration with different doses of 5, 10 and 20   mg/kg.

研究领域: 分析化学 · 药物代谢动力学 · 毒理学
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2023 · IF 6

Magnetic covalent organic framework for effective solid-phase extraction and HPLC determination of ochratoxin A in food

Xiao-Shuai Yang,Jie Zhao,Tian-Tian Ma,Zi-Yu Li,Lu-Liang Wang,Shi-Lei Ji,Meng-Yue Sun,Yu-Shen Liu,Zhen-Hua Hu,Quan-Wen Liu,Cheng-Wu Jin,Shu-Yang Sun,Han-Sheng Gong

Ochratoxin A (OTA) exposure in food poses great threat to human health. Magnetic solid phase extraction (MSPE) is an effective sample pre-treatment method based on liquid chromatographic analysis to monitor OTA in food. Herein, magnetic covalent organic frameworks (Fe 3 O 4 @COFs) nanospheres were prepared and well characterized. The efficient and selective extraction of OTA relied on large specific surface and inherent porosity of COFs and the hydrogen bonding, π-π and hydrophobic interactions between COF shell and OTA. The MSPE parameters were investigated in detail. Under the optimal MSPE conditions, the developed Fe 3 O 4 @DhaTab-based-MSPE-HPLC-FLD method for OTA displayed good linearity (0.1-800 μg L −1 ) with R 2 (0.996) and low limit of detection (0.03 μg L −1 ). The proposed method was applied to determine OTA in beer, Chinese Baijiu and vinegar with satisfactory recoveries (72–111%) and relative standard deviations (0.2 to 5.5%).

✓ 已验证 产品关联 DOI 高影响因子
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Evidence-based Complementary and Alternative Medicine · 2023 · IF 2.65

Online Microextraction Coupled with HPLC-ABTS for Rapid Analysis of Antioxidants from the Root of Polygonum bistorta

Wei-Qi Yang,Zheng-Ming Qian,Meng-Qi Wu,Jian-Li Gao,Qi Huang,Yuan-Sheng Zou,Dan Tang

The root of Polygonum bistorta (PB) is a traditional Chinese medicinal plant material widely used in China. It has been commonly used for the treatment of hemostasis, detumescence, diarrhea, snake bite, and acute gastroenteritis. However, the research on the antioxidant properties and bioactive compounds from PB is inadequate. In the current research, an online microextraction (OLME) coupled with a high-performance liquid chromatography coupled with the 2,2-nitrogen-di (3-ethyl-benzothiazole-6-sulfonic acid) diammonium salt antioxidant assay (HPLC-ABTS) system for rapid analysis of antioxidants from PB was proposed. The PB sample (0.17 mg) was online extracted by mobile phase (acetonitrile and 0.2% acetic acid); a Poroshell 120 SB-Aq column was used for separation; then, an online ABTS assay system was used for screening the antioxidants. Finally, ten components were found in PB, and among them, eight components possessed antioxidant activities. Furthermore, five components (gallic acid, neochlorogenic acid, caffeic acid, chlorogenic acid, and an unknown compound) were proved as major antioxidants when compared with rutin as an antioxidant marker. The results showed that the developed OLME-HPLC-ABTS system was a simple, rapid, green, and efficient instrument for the screening of antioxidants from PB, which provides a powerful tool for the discovery of natural antioxidants in Chinese medicines.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2023 · IF 4.3

HPLC-MS/MS method for the simultaneous determination of lysine-derived markers for protein carbonylation in meat

Shouyin Wang,Shengjie Li,Wenhui Wang,Xiuxia Guo,Jinfeng Pan,Xiuping Dong

This paper aimed to develop a quantitative method based on high-performance liquid chromatography (HPLC) coupled with triple quadrupole tandem mass spectrometry (MS/MS) for the simultaneous determination of two protein carbonylation products derived from lysine residues in meat proteins, namely, α-aminoadipic semialdehyde (AAS) and lysinonorleucine (LNL). Mass spectrometry conditions and derivatization parameters were optimized and the linearity, repeatability, bias, the limit of detection (LOD), the lower limit of quantification (LLOQ), and recovery were validated. The developed method showed satisfactory linearity, repeatability, and sensitivity for both AAS and LNL. This method was applied to analyze the contents of these compounds in different meat products, and the formation of AAS was observed to be closely related to the severity of the manufacturing conditions. Moreover, AAS was demonstrated to be a reliable but more sensitive marker for protein carbonylation compared to the DNPH method, which could also provide information regarding the specific pathway of protein carbonylation.

✓ 已验证 产品关联 DOI 高影响因子
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MICROCHEMICAL JOURNAL · 2022 · IF 5.304

Determination of synthetic estrogens in milk by a novel hyper-crosslinked polymer SPME coupled with HPLC-MS

Tong Liao,Jia Jia,Kang Tong,Jiuhong Ouyang,Wei Jiang,Xia-ping Zhu

A novel hyper-crosslinked 2, 8, 14, 20-tetraphenyl calix [4] resorcinol arene polymer (HCP-TCRA) was synthesized by using an external crosslinking of 2, 8, 14, 20-Tetraphenyl calix [4] resorcinol arene (TCRA) as monomers and dimethoxymethane as crosslinker. The HCP-TCRA was explored as a SPME fiber coating material. A variety of physicochemical characterization demonstrated that the material has excellent chemical/thermal stability and strong hydrophobicity. The fiber demonstrated fantastic adsorptive property for three synthetic estrogens (diethylstilbestrol, hexestrol, ethinyloestradiol, abbreviated to SESs). In this work, an efficient HCP-TCRA fiber-based SPME method was developed to analyze SESs by coupling with HPLC-MS detection. Under the optimized SPME conditions, this method was shown a wide range of linearity (2.0–100.0 ng mL −1 for diethylstilbestrol, 1.0–100.0 ng mL −1 for hexestrol, and 30.0–480.0 ng mL −1 for ethinyloestradiol), low limits of detection (LODs, 0.5 ng mL −1 for DES 0.3 ng mL −1 for HEX, 10.0 ng mL −1 for EES) and fine reusability (more than 30 times). Finally, the proposed methods had been applied to the determination of SESs in milk samples with a simple pretreatment. At three different levels, relative recoveries presented between 86.7 and 106.4%. The method put up highly sensitive and budget-friendly   in detection SESs, and has capacity in quality control of milk products.

CAS / MDL: 56-53-1
✓ 已验证 产品关联 DOI 高影响因子
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JOURNAL OF FOOD SCIENCE · 2022 ·Vol. 87 ·期 4 ·1575-1585 · IF 3.693

Extraction and detection of morin from Sanghuangporus lonicericola by magnetic molecularly imprinted polymers coupled with HPLC analysis

Wei Zhang,Yunjing Luo,Ziqi Xie,Chenchen Kong,Zhen Na

In this study, morin magnetic molecularly imprinted polymers (Morin-MMIPs) were synthesized based on magnetic nanoparticles and surface molecularly imprinted technology with superparamagnetism and extraction selectivity. The polymers allowed the separating of morin from complex matrices in the presence of an external magnetic field with no need for centrifugation or filtration. The microstructure of the polymers was characterized by scanning electron microscopy and transmission electron microscopy. Meanwhile, the functional group and magnetic properties of the polymers were characterized using Fourier transform infrared spectroscopy (FT-IR) and magnetic vibration meter (VSM). The maximum adsorption capacity of MMIPs was 3.24 mg/g, which was 2.55 times higher than that of MNIPs (1.27 mg/g). Morin was quantified by HPLC-DAD, which showed good linearity in the concentration range of 0.05–60 µg/ml with the correlation coefficient R 2 = 0.9993. The limit of detection (LOD) was 0.08 µg/ml, and the spiked recoveries were 87.5–106.8%. The calculation of the adsorption isotherm and kinetic model revealed the adsorption mechanisms, and the adsorption process was consistent with the Langmuir adsorption isotherm and pseudo-secondary kinetic models. Likewise, the material has been successfully used to extract and separate morin from food samples. The method reported in this paper has the advantages of fast adsorption speed, high selectivity, and environmental friendliness. It provided a reliable method for the separation and detection of morin or other natural products.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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RSC Advances · 2021 ·Vol. 11 ·期 63 ·39821-39828 · IF 3.361

Boronate-modified polyethyleneimine dendrimer as a solid-phase extraction adsorbent for the analysis of luteolin via HPLC

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.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD CHEMISTRY · 2021 · IF 7.514

Rapid determination of 2,4-diaminopyrimidine residues through sample pretreatment using immunomagnetic bead purification along with HPLC–UV

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.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF MOLECULAR STRUCTURE · 2022 · IF 3.841

HPLC, fluorescence spectroscopy, UV spectroscopy and DFT calculations on the mechanism of scavenging •OH radicals by Hypericin

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.

CAS / MDL: 5144-89-8
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FOOD CHEMISTRY · 2020 · IF 6.306

HPLC-DAD fingerprints combined with chemometric techniques for the authentication of plucking seasons of Laoshan green tea

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.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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