MICROCHIMICA ACTA
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2019
·Vol. 186
·期 4
·1-9
·
IF 5.479
Tong Yao,Liu Xueyan,Zhang Lei
Magnetic porous microspheres composed of Fe 3 C, MnO and graphitic carbon (Fe 3 C/MnO/GC) were prepared by a one-pot method. A polycondensate obtained from urea and formaldehyde served as the carbon source and was calcined in the presence of metallic iron and manganese to yield Fe 3 C/MnO/GC. The resultant hybrid has highly mesoporous architecture, large specific surface, graphitic structure and adequate saturation magnetism. It is shown to possess excellent pre-concentration ability for herbicides (monuron, chlortoluron, atrazine and terbutylhylazine). The sorbent can be easily separated and has a long service lifetime (>25 cycles). Under optimized conditions, the sorbent excels by good recoveries (78–120%), high enrichment factors (45–50) and good precision (RSDs ≤10.7%). The limits of detection are 0.01–0.10 μg L −1 for (spiked) water samples, 0.22–0.87 μg kg −1 for grape samples, and 0.18–0.74 μg kg −1 for potato samples. This work offers a new strategy for the construction of magnetic bimetallic heterostructured GC hybrids.
Schematic presentation of magnetic porous Fe 3 C/MnO/graphitic carbon microspheres and their application for the enrichment of trace level herbicides prior to HPLC analysis.
研究领域:
材料科学
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环境科学
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分析化学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2016
·
IF 3.169
Yidi Yang,Xi Zhu,Fei Zhang,Wei Li,Ying Wu,Li Ding
Stress testing was carried out under acidic, alkaline, oxidative, thermal and photolytic conditions to evaluate the intrinsic stability of posaconazole injection. A total of four degradation products were detected and the drug was found to be susceptible to oxidative and thermal degradations. Three unknown degradants formed under oxidative stress condition were isolated by preparative HPLC and unambiguously elucidated by LC–TOF/MS, LC–MS/MS, 1 H NMR, 13 C NMR and 2D NMR techniques. Based on the spectrometric and spectroscopic information, these novel degradation products were unequivocally assigned as the N-oxides of posaconazole. Probable mechanisms for the formation of the degradants were proposed. A new and selective HPLC method was developed and validated to separate, detect and quantify all the degradants in posaconazole injection.
研究领域:
药物分析
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药学
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质谱分析
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核磁共振
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DOI
PubMed
高影响因子
International Journal of Analytical Chemistry
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2022
·
IF 1.698
Lijing Li,Kaixuan Zhou,Qiulu Zhao,Yuejie Wang,Jia Liu,Huiwei Bao
Buyang Huanwu Decoction (BHD) has lipid-lowering and antioxidant effects. In this study, HPLC was used to establish the fingerprint of extracts from different polar parts of BHD. Through the L02 cell lipid deposition model induced by oleic acid, extracts from different polar parts of BHD were administered for treatment. Oil red O staining, TG detection, and MDA detection were used to determine lipid deposition and antioxidant activity. The component-effect relationship is established by using grey relational analysis and PLSR analysis. The results showed that the extracts from different polar parts of BHD could reduce the levels of TG and MDA. The grey relational analysis showed that the peaks that contributed greatly to the reduction of TG and MDA were peaks 3, 16, 14, 10, 1, 15, 2, and 11, respectively. Peaks 1, 4, 9, 10, 14, 16, and 17 could reduce TG and MDA through PLSR analysis. According to the results of grey relational analysis and PLSR analysis, peaks 1, 10, 14, and 16 may have good lipid-lowering and antioxidant effects. This study provides a certain preliminary basis for follow-up research on lipid-lowering drugs.
研究领域:
药理学
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生物化学
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中医药
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DOI
PubMed
高影响因子
MOLECULES
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2020
·Vol. 25
·期 19
·4507
·
IF 3.267
Zhen Li,Zongcai Tu,Hui Wang,Lu Zhang
Ceratophyllum demersumL. (CDL) is a traditional Chinese herb to treat many diseases, but research on its anti-diabetic activity is not available. In this research, the α-glucosidase inhibitory ability and phytochemical constituents of CDL extract were firstly studied. Optimal ultrasound-assisted extraction conditions for α-glucosidase inhibitors (AGIs) were optimized by single factor experiment and response surface methodology (RSM), which was confirmed as 70% methanol, liquid-to-solid ratio of 43 (mL/g), extraction time of 54 min, ultrasonic power of 350 W, and extraction temperature of 40 °C. The lowest IC50value for α-glucosidase inhibition was 0.15 mg dried material/mL (mg DM/mL), which was much lower than that of acarbose (IC50value of 0.64 mg DM/mL). In total, 80 compounds including 8 organic acids, 11 phenolic acids, 25 flavonoids, 21 fatty acids, and 15 others were identified or tentatively identified from CDL extract by HPLC-QTOF-MS/MS analysis. The results suggested that CDL could be a potential source of α-glucosidase inhibitors. It can also provide useful phytochemical information for research into other bioactivities.Keywords:Ceratophyllum demersumL.;response surface methodology;α-glucosidase inhibitors;phytochemical profile
研究领域:
药理学
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植物化学
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中药学
✓ 已验证
DOI
PubMed
高影响因子
Analytical Methods
·
2018
·Vol. 11
·期 1
·105-112
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IF 2.073
Peige Qin,Yixin Yang,Wenqi Li,Jing Zhang,Qian Zhou,Minghua Lu
In this work, amino-functionalized mesoporous silica nanospheres (MSN-NH2) were synthesized and demonstrated as useful sorbents of dispersive solid-phase extraction (dSPE) for extraction and preconcentration of synthetic dyes (tartrazine, amaranth, sunset yellow, allura red, and orange II) from foodstuffs prior to high-performance liquid chromatography (HPLC) analysis. The MSN-NH2 was characterized by transmission electron microscopy, Fourier-transform infrared spectroscopy, nitrogen adsorption and desorption isotherms, and elemental analysis. To achieve optimized extraction efficiency, several critical factors including amount of MSN-NH2, sample pH, adsorption time, adsorption temperature, desorption time, and desorption solvents, were systematically investigated. Under the optimized conditions, the enrichment factors were higher than 120. The limits of detection were found to be 0.10–0.30 ng mL−1. The method showed excellent linearity in the range of 0.45–1000.0 ng mL−1 with correlation coefficients (R2) ≥ 0.9951. The intra-day and inter-day precision (n = 5) were 1.72–3.64% and 1.45–4.52%. The recoveries at three concentration levels ranged from 82.7 to 116.3%. The proposed dSPE by using MSN-NH2 as sorbent coupled with HPLC was successfully applied to the analysis of synthetic dyes in real samples.
研究领域:
分析化学
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食品安全
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材料科学
✓ 已验证
DOI
高影响因子
Journal of Food Measurement and Characterization
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2021
·Vol. 15
·期 5
·3873-3883
·
IF 2.431
Qian Zheng-ming,Huang Qi,Feng Xiao-long,Li De-qiang
Given the safety of synthetic antioxidants, people are increasingly inclined to develop and use natural antioxidants. However, rapid screening and identification of active ingredients from the complex systems of natural products is one of the major challenges for the modernization of traditional Chinese medicine. In this study, online extraction-high performance liquid chromatography-diode array detection-quadrupole time-of-flight mass spectrometry coupled with ABTS antioxidant assay (OLE-HPLC-DAD-QTOF-MS/MS-ABTS), in which sample preparation, separation, detection and antioxidant assay were integrated in a single step, was used to rapidly identify antioxidant components from the different parts of Citrus reticulata , including its peels, leaves, vascular bundies and seeds. After method validation (system adaptability, extraction yield and repeatability), the four samples of different botanical parts were analyzed. As a result, among 49 found chromatographic peaks, 33 peaks displayed varying degrees of antioxidant activity and 39 peaks were tentatively or unambiguously identified based on their retention time, UV spectrum and mass spectrometry information and the comparison with reference substance and data in literature, including 10 phenolic acids, 9 polymethoxy flavonoids, 7 flavonoid- O -glycosides and 13 other ingredients. It is concluded that the established method is simple, fast, and reliable, which not only saves the materials and solvents as well as time, but also reduces the risk of degradation of chemical components during the extraction process, suitable for rapid screening and identification of antioxidant components of complex mixture.
研究领域:
生药学
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分析化学
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天然产物
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中药学
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产品关联
DOI
高影响因子
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.
研究领域:
环境科学
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分析化学
·
毒理学
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产品关联
DOI
PubMed
高影响因子
TALANTA
·
2017
·
IF 4.162
Rui Xiao,Xiaoting Zhang,Xiaona Zhang,Jiahua Niu,Minghua Lu,Xiuhua Liu,Zongwei Cai
In this article, a method for the analysis of flavors and fragrances including ethyl vanillin , trans-cinnamic acid, methyl cinnamate , ethyl cinnamate , and benzyl cinnamate in foods by HPLC with Fe 3 O 4 @GO nanocomposite as the adsorbent of magnetic solid-phase extraction was developed. The magnetic Fe 3 O 4 @GO nanocomposite was prepared and characterized by transmission electron microscope, infrared spectroscopy , X-ray diffraction and vibrating sample magnetometer. The as-prepared Fe 3 O 4 @GO nanocomposite was used as adsorbent for extraction and preconcentration of flavors and fragrances in foods. The extraction and desorption conditions including amount of materials, extraction time and desorption solvents were investigated. The analytes were separated within 10 min and detected with LODs ranged from 0.02 to 0.04 μg/mL. The recovery obtained from the analysis of spiked juice sample was between 71.5% and 112.4% with RSDs lower than 4.14%. The developed method was successfully applied to the analysis of real samples including orange juice, chocolate and fruit sugar.
研究领域:
分析化学
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食品科学
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产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2016
·Vol. 8
·期 6
·1405-1414
·
IF 1.915
Na Cao,Lei Liu,Yuan-bin Hao,Li-li Sun,Qiao-gen Zou,Xing-ling Ma,Kai-he Xiong
A sensitive, rapid and stable HPLC-MS/MS method has been developed and validated for the determination of rabeprazole enantiomers and their four metabolites, namely rabeprazole thioether, rabeprazole sulfone and desmethyl rabeprazole enantiomers, in beagle dog plasma using esomeprazole as the internal standard. The analytes and the internal standard were extracted from plasma samples by liquid–liquid extraction and separated on a Chiral-HSA column using acetonitrile-10 mmol L−1 ammonium acetate as the mobile phase by gradient elution. The method was validated with respect to sensitivity, specificity, linearity, precision, accuracy and especially the stability of analytes under various conditions, and was successfully applied in evaluating the pharmacokinetic profiles of racemic rabeprazole, the pure enantiomers and their metabolites in beagle dogs after single intravenous administration of (R)-rabeprazole sodium injection (at 0.33, 1 and 3 mg kg−1), (S)-rabeprazole sodium injection (at 1 mg kg−1) and racemic rabeprazole sodium injection (at 2 mg kg−1). The two enantiomers showed different profiles of pharmacokinetic parameters. The AUC0–t and t1/2 values of (R)-rabeprazole were higher and the clearance (CL) value of (R)-rabeprazole was lower than that of (S)-rabeprazole. Compared to (S)-rabeprazole, the higher absorption and slower elimination of (R)-rabeprazole explain why (R)-rabeprazole is more effective than the racemate.
研究领域:
药物分析
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药理学
·
临床医学
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产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Fukai Li,Min Wang,Jian Zhou,MengRui Yang,TongTong Wang
A novel cyclodextrin-derivatized hybrid magnetic nanocomposite, denoted as Fe 3 O 4 @SiO 2 @CD, was fabricated and employed as the adsorbent of magnetic solid-phase extraction (MSPE) for preconcentration of elven fluoroquinolones (FQs) from water samples. The prepared nanoparticles exhibited excellent magnetic responsiveness (56.7 emu g −1 ), uniform size distribution (about 300 nm), good thermal and chemical stability, excellent reusability and superior chemical affinities to the target FQs via hydrogen bond, host–guest inclusion complexation and π–π interactions. Under the optimized conditions, the MSPE was coupled with HPLC-MS/MS to sensitively quantify trance levels of FQs in environmental water. The developed method revealed satisfactory precision with RSDs lower than 4%, good linearity (R 2 ≥ 0.9981), low limits of detection (0.0014–0.023 µg L −1 ) and satisfactory recoveries (93.2–105%). Furthermore, the proposed approach was validated by analyzing the Certified Reference Material of GBW 10152 and GBW 10153 chicken meat powder. These results demonstrated that the Fe 3 O 4 @SiO 2 @CD nanoparticles are a promising magnetic adsorbent for FQs, and the established MSPE-HPLC-MS/MS approach is suitable for simultaneous analysis of trace levels of FQs in actual samples.
研究领域:
分析化学
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环境科学
·
药物分析
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产品关联
DOI
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2020
·Vol. 412
·期 30
·8339-8350
·
IF 3.637
Gao Yue,Tan Jiangkun,Lu Jiao,Sun Zhiwei,Li Zan,Ji Zhongyin,Zhang Shijuan,You Jinmao
In this study, a novel fluorescent labeling reagent 2-(9-acridone)-ethyl chloroformate (AEC-Cl) was designed, synthesized and applied for the determination of free amino acids by high-performance liquid chromatography with a fluorescence detector (HPLC-FLD). The free amino acids were rapidly and efficiently labeled by AEC-Cl in the presence of basic catalyst (pH 9.0) within 5 min at room temperature (25 °C). The derivatives exhibited excellent stability and fluorescence properties, with maximum excitation and emission wavelengths at 268 nm and 438 nm, respectively. Derivatives of 22 kinds of natural amino acids were completely separated by gradient elution on a Hypersil ODS C18 column. Under the optimal conditions, the calibration curves exhibited excellent linear responses, with correlation coefficients of R 2 > 0.9994. The detection and quantification limits were in the range of 0.61–2.67 μg kg −1 and 2.07–8.35 μg kg −1 , respectively. Therefore, AEC-Cl was successfully applied for the detection of trace levels of free amino acids in honey samples.
A novel fluorescent labeling reagent was applied for the determination of free amino acids in honey by high-performance liquid chromatography with a fluorescence detector.
研究领域:
分析化学
·
食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2024
·
IF 8.5
Ruidong Zhou,Yupeng Wen,Wendi Huo,Cong Kong,Guangxin Yang,Huan Liu,Chaoying Zhang,Yingchun Mu,Dongmei Huang,Jincheng Li
A modified QuEChERS method was developed to determine multi-class pesticide and veterinary residues in aquatic products. Chitosan microspheres were conveniently synthesized and utilized as the cleanup adsorbent in the QuEChERS procedure, showcasing rapid filtration one-step pretreatment ability for the determination of drug multi-residues in aquatic products. Compared to conventional synthetic sorbents, chitosan microspheres not only have good purification performance, but also have renewable and degradable properties. This novel sorbent worked well in the simultaneous determination of 95 pesticides and veterinary drug residues in aquatic products after being combined with an improved one-step vortex oscillating cleanup method. We achieved recoveries ranging from 64.0% to 115.9% for target drugs in shrimp and fish matrix. The limits of detection and quantification were 0.5–1.0 and 1.0–2.0 μg kg −1 , respectively. Notably, hydrocortisone was detected with considerable frequency and concentration in the tested samples, underscoring the necessity for stringent monitoring of this compound in aquatic products.
研究领域:
分析化学
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环境科学
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）