JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2019
·
IF 2.813
Zheng-ming Qian,Ling Chen,Meng-qi Wu,De-qiang Li
Rapid discovery of active ingredients from complex matrices is one of great challenges for modern drug development. Traditional methods often require many sample treatment steps, including an extraction step with exclusively dedicated solvents followed by repeated separation and activities assessment. This present work described an integrated analytical setup for natural antioxidants discovery in which the online extraction (OLE) of a solid sample is directly coupled to its analysis by high performance liquid chromatography-diode array detector-quadrupole time-of-flight tandem mass spectrometry and 2,2′-Azinobis-(3-ethylbenzthiazoline-6-sulphonate) (ABTS) antioxidant assay (OLE-HPLC-DAD-QTOF-MS/MS-ABTS). This developed approach makes sample extraction, chromatographic separation and chemical detection, and antioxidant assay integrated into a single HPLC injection and was successfully applied for the rapid discovery of natural antioxidant bioactives from Polygonum viviparum . A total of 21 secondary metabolites were characterized according to their retention times, ultraviolet (UV) spectra, exact mass and fragmentation ions in MS/MS spectra, and 18 of them displayed antioxidant activity (response as negative peaks in antioxidant assay). This work describes a simple, green and efficient approach to minimize the sample consumption (only 0.4 mg was required) and eliminate complex sample treatment procedures. The developed OLE-HPLC-DAD-QTOF-MS/MS-ABTS system offers new perspectives for rapid chemical profiling of natural products and their antioxidants discovery.
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高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2023
·
IF 3
Rong-Fa Xu,Hang Mei,Li Chen,Bin Tang,Qi-Yuan Lu,Feng-Shan Cai,Xiao Yan,Jing Zheng,Xian-Tao Shen,Yun-Jiang Yu
Humans are widely and concurrently exposed to volatile organic compounds (VOCs) and polycyclic aromatic hydrocarbons (PAHs). However, few studies have reported the internal co-exposure levels of these chemicals in occupational and general populations. Specifically, the associations revealed between the urinary levels of metabolites of VOCs (mVOCs), hydroxylated PAHs (OH-PAHs), and oxidative stress biomarkers for humans remain limited. In this study, a method based on solid-phase extraction (SPE) and liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous analysis of 22 mVOCs, 12 OH-PAHs, and 8-hydroxy-2′-deoxyguanosine (8-OHdG) in human urine samples. The method was validated with all target analyte accuracies and precisions in the range of 76 %–120 % and 1 %–14 % at three levels of spiked urine samples, respectively. The limit of detection (LOD) and limit of quantification (LOQ) of the target analytes were 0.01–0.34 ng/mL and 0.01–7.57 ng/mL, respectively. And the method was applied to measure urinary levels of target analytes from 38 petrochemical workers in Guangzhou, South China. Except for 3-hydroxy-benzo[a]pyrene, all target analytes were detected in the urine samples. The average levels were 0.05–12.6 ng/mL for individual OH-PAHs, 0.20–73620 ng/mL for individual mVOCs, and 1.00 ng/mL for 8-OHdG. Additionally, 3-hydroxy-phenanthrene, 1-hydroxy-pyrene, 6-hydroxy-chrysene, N-acetyl-S-(trichlorovinyl)-L-cysteine, 2-methylhippuric acid, thiodiacetic acid, trans, trans -Muconic acid, and N-acetyl-S-(3,4-dihydroxybutyl)-L-cysteine had statistically significant positive effects on 8-OHdG levels, while 1-hydroxy-naphthalene, 1,2-dihydroxybenzene, and hippuric acid showed a negative effect on 8-OHdG, indicating these metabolites could lead to synergistic or antagonistic oxidative DNA damage. This study provides a robust analytical method that permits a comprehensive assessment of co-exposure to PAHs and VOCs and their potential adverse health effects.
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高影响因子
MOLECULES
·
2023
·Vol. 28
·期 14
·5309
·
IF 4.6
Shi-Hui Lu,Xiao-Na Liang,Xiao-Jin Nong,Ran Chen,Xiu-Xia Li
Trans-p-hydroxycinnamic acid and its esters in the leaves ofLigustrum robustummight be a new resource to prevent diabetes and its complications. In the present study, a new HPLC-UV method using hydrolyzation with sodium hydroxide for quantitation oftrans-p-hydroxycinnamic acid and totaltrans-p-hydroxycinnamic acid esters in the leaves ofL. robustumwas developed, since it was difficult and troublesome to analyze no less than 34trans-p-hydroxycinnamic acid esters by usual HPLC. The extract ofL. robustumwas hydrolyzed with sodium hydroxide at 80 °C for 2 h, and then, hydrochloride was added. HPLC analysis was performed in reverse phase mode using a C-18 column, eluting with methanol-0.1% acetic acid aqueous solution (40:60,v/v) in isocratic mode at a flow rate of 1.0 mL·min−1and detecting at 310 nm. The linear range fortrans-p-hydroxycinnamic acid was 11.0–352.0 μg·mL−1(r2= 1.000). The limit of detection and limit of quantification were 2.00 and 6.07 μg·mL−1, respectively. The relative standard deviations of intra-day and inter-day variabilities fortrans-p-hydroxycinnamic acid were less than 2%. The percentage recovery oftrans-p-hydroxycinnamic acid was 103.3% ± 1.1%. It is the first HPLC method using hydrolyzation for quantification of many carboxylic esters. Finally, the method was used successfully to determinetrans-p-hydroxycinnamic acid and totaltrans-p-hydroxycinnamic acid esters in various extracts of the leaves ofL. robustum. The 60–70% ethanol extracts ofL. robustumshowed the highest contents of freetrans-p-hydroxycinnamic acid (3.96–3.99 mg·g−1), and the 50–80% ethanol extracts ofL. robustumdisplayed the highest contents of totaltrans-p-hydroxycinnamic acid esters (202.6–210.6 mg·g−1). The method can be applied also to the quality control of the products ofL. robustum.Keywords:trans-p-hydroxycinnamic acid;esters;Ligustrum robustum;HPLC-UV;hydrolyzation;sodium hydroxide;quantification
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INTERNATIONAL JOURNAL OF FOOD SCIENCE AND TECHNOLOGY
·
2018
·Vol. 53
·期 6
·1494-1502
·
IF 2.383
Fang-Fang Chen,Jie Sang,Yao Zhang,Jun Sang
Summary This study aimed to develop a green two-dimensional HPLC-DAD/ESI-MS method for analysing anthocyanins from Prunus cerasifera var. atropurpurea leaf and improve their stability in energy drinks by the addition of phenolic acids. Ethanol and tartaric acid solutions were used as mobile phases for one-dimensional HPLC-DAD for quantitative analysis of anthocyanins, and the primary anthocyanins were identified as cyanidin-3- O -galactoside, cyanidin-3- O -glucoside and cyanidin-3- O -rutinoside using two-dimensional HPLC-MS. Method validation showed that the developed method was accurate, stable and reliable for the analysis of P. cerasifera anthocyanins. The effects of gallic, ferulic and caffeic acid on the stability of cyanidin-3- O -galactoside, cyanidin-3- O -glucoside, cyanidin-3- O -rutinoside and total anthocyanins from P. cerasifera leaf in energy drinks were evaluated, and the degradation of P. cerasifera anthocyanins ideally followed a first-order model ( R 2 > 0.98). Gallic acid showed stronger protective effects on P. cerasifera anthocyanins in energy drinks, and adding/increasing ferulic and caffeic acids accelerated the degradation reactions.
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JOURNAL OF SEPARATION SCIENCE
·
2016
·Vol. 39
·期 10
·1971-1978
·
IF 2.741
Xiaozhong Wang,Xuwen Li,Lanjie Li,Min Li,Ying Liu,Qian Wu,Peng Li,Yongri Jin
A simple and sensitive method for determination of three aconitum alkaloids and their metabolites in human plasma was developed using matrix solid-phase dispersion combined with vortex-assisted dispersive liquid–liquid microextraction and high-performance liquid chromatography with diode array detection. The plasma sample was directly purified by matrix solid-phase dispersion and the eluate obtained was concentrated and further clarified by vortex-assisted dispersive liquid–liquid microextraction. Some important parameters affecting the extraction efficiency, such as type and amount of dispersing sorbent, type and volume of elution solvent, type and volume of extraction solvent, salt concentration as well as sample solution pH, were investigated in detail. Under optimal conditions, the proposed method has good repeatability and reproducibility with intraday and interday relative standard deviations lower than 5.44 and 5.75%, respectively. The recoveries of the aconitum alkaloids ranged from 73.81 to 101.82%, and the detection limits were achieved within the range of 1.6–2.1 ng/mL. The proposed method offered the advantages of good applicability, sensitivity, simplicity, and feasibility, which makes it suitable for the determination of trace amounts of aconitum alkaloids in human plasma samples.
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高影响因子
MOLECULES
·
2014
·Vol. 19
·期 4
·4857-4879
·
IF 2.095
Chen Li,Feng Xu,De-Mei Xie,Yu Jing,Ming-Ying Shang,Guang-Xue Liu,Xuan Wang,Shao-Qing Cai
Traditional Chinese Medicine (TCM) nasal therapy has been utilized to treat numerous diseases for over two millennia. It has many advantages compared with other routes. In this article, headspace-solid phase microextraction-gas chromatography-mass spectrometry and high performance liquid chromatography-atmospheric pressure chemical ionization-ion trap-time of flight-multistage mass spectrometry were applied for the first time to analyze the absorbed constituents in rabbit plasma and cerebrospinal fluid (CSF) after intranasal administration of Asari Radix et Rhizoma (AR). In total, 47 absorbed AR constituents including 14 monoterpenes, 10 phenylpropanoids, four benzene derivatives, two alkanes, nineN-alkylamides and eight lignans were tentatively identified in the rabbit plasma and CSF. Thirty-three absorbed constituents are found to have different bioactivities related to the pharmacological actions of AR through bibliography data retrieval. These indicated that many types of constituents of TCM can be absorbed at the nasal cavity into both rabbit blood and CSF. This is the first study to explore the absorption of AR, and comprehensively analyze the absorbed constituents after intranasal administration of TCM. These findings extend our understanding of the effective substances of AR, and inspire us to make a hypothesis on the mechanism of additive effect of multiple constituents of TCMs, which is very worthy of further investigation.Keywords:nasal therapy;Asarum heterotropoidesvar.mandshuricum;intranasal administration;effective substance;cerebrospinal fluid;absorption;SPME;GC-MS;LC-MS;additive effect
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JOURNAL OF HAZARDOUS MATERIALS
·
2024
·
IF 12.2
Jinling Pang,Hongzhe Chen,Huige Guo,Kunning Lin,Shuyuan Huang,Beichen Lin,Yuanbiao Zhang
Microplastics (MPs) act as carriers for organic pollutants ( e.g. antibiotics) and microorganisms ( e.g. bacteria) in waters, leading to the proliferation of antibiotic resistance genes. Moreover, the antibiotics adsorbed on MPs may exacerbate this process. For further research, it is necessary to understand the types and amounts of antibiotics adsorbed on MPs. However, due to the heavy work of MPs collection and sample pretreatment, there is a lack of analytical methods and relevant data. In this study, an in-tube solid phase microextraction (IT-SPME) on-line coupled to HPLC-MS/MS method based on amorphous precursor polymer of three-dimensional covalent organic frameworks/monolith-based composite adsorbent was developed, which could efficiently capture, enrich and analyze tetracycline (TCs) antibiotics. Under the optimal extraction parameters, the developed method was capable of detecting TCs at levels as low as 0.48–1.76 pg. This method was applied to analyze the TCs adsorbed on MPs of different particle sizes in mariculture water for the first time, requiring a minimum amount of MPs of only 1 mg. Furthermore, it was observed that there could be an antagonistic relationship between algal biofilm and TCs loaded on MPs. This approach could open up new possibilities for analyzing pollutants on MPs and support deeper research on MPs.
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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.
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JOURNAL OF SEPARATION SCIENCE
·
2023
·
IF 3.1
Wei-Qi Yang,Qi Huang,Meng-Qi Wu,Quan-Xi Mei,Yuan-Sheng Zou,Zheng-Ming Qian,Dan Tang
To reveal the utilization value of leaf, stem, and root of Artemisia argyi , a rapid online liquid microextraction combined with a high-performance liquid chromatography coupled with 2,2-nitrogen-di (3-ethyl-benzothiazole-6-sulfonic acid) diammonium salt antioxidant assay system was established for analysis of antioxidants in the leaf, stem, and root of A. argyi , and a calibration quantitative method of antioxidant activity with equivalent chlorogenic acid was proposed. Thirty-three positive peaks were identified; among them, 12 compounds were found that possess good antioxidant activity including eleven organic acids (components 2–4, 8, 11–14, 17, 19, and 21) and one flavonoids (component 22). The proposed calibration quantitative method avoided the influence of content of compound and compared the extent of radical scavenging capacity of five antioxidant compounds, which were ranked as follow: 3,5-dicaffeoylquinic acid > 3,4-dicaffeoylquinic acid ≈ 4,5-dicaffeoylquinic acid > 1,4-dicaffeoylquinic acid > chlorogenic acid. In conclusion, this study provided composition and biological potential for the future development of the leaf, stem, and root of A. argyi . It is believed that the online liquid microextraction combined with high-performance liquid chromatography based antioxidant assay system can be widely used for the rapid screening of natural antioxidant components in the different parts of natural products.
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高影响因子
MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 6
·1-11
·
IF 5.479
Chen Zhipeng,Yu Chen,Xi Jiangbo,Tang Sheng,Bao Tao,Zhang Juan
A hybrid material was synthesized by growing a covalent organic framework (COF) in-situ on the surface of functionalized metal organic framework (MOF). Specifically, the amino-modified MOF (type MIL-68) was obtained by reacting indium(III) nitrate and 2-aminoterephthalic acid. Subsequently, it was reacted with tris(4-formylphenyl)amine and tris(4-aminophenyl)amine to obtain the final hybrid COF. This material overcomes the disadvantage of MOF concerning poor stability in aqueous solution and it combines the advantages of MOF and COF. This MOF@COF hybrid material is shown to be a viable adsorbent for the extraction of sulfonamides by pipette tip solid-phase extraction). Following elution with acetonitrile, the sulfonamides were quantified by high performance liquid chromatography using variable wavelength detection (HPLC-VWD). The structure and morphology of the material was characterized by various techniques. Extraction parameters such as amount of adsorbent, sampling rate, sample pH, elution solvent and sample volume were investigated. Under the optimum conditions, the sulfonamides tested (sulfadimethoxine sulfamethoxazole, sulfamonomethoxine, sulfamethazine, sulfamerazine and sulfadiazine) can be determined over a wide linear range (10–2000 ng·mL −1 ), with low limits of detection (1 ng·mL −1 ) and high precision (RSD <5.2%). The method was applied the determination of sulfonamide residues in (spiked) environmental water, milk and meat samples and gave recoveries in the range from 68.9–103.8%, with RSDs of <6.6%. The packed pipette tip column exhibits excellent stability, reproducibility and high adsorption capacity.
A hybrid sorbent was prepared by controlled growth of a covalent organic framework on amino-modified MIL-68 and packed into a pipette tip for sulfonamide extraction. The sensitivity was dramatically increased after optimized extraction, with limit of detection as low as 1 ng·mL -1
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Food Bioscience
·
2025
·
IF 5.9
Lu Feng,Jingxia Yang,Liping Sun,Xiaoyan Zhu,Wei Lan,Guangqing Mu,Xuemei Zhu
We evaluated the changes in volatile and nonvolatile flavor substances after fermented milk was fermented by Lacticaseibacillus rhamnosus WH. FH-19 using Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS) and High-Performance Liquid Chromatography-Mass Spectrometry (HPLC-MS). The results have shown that the addition of L. rhamnosus WH. FH-19 can increase the contents of acetoin and 2-nonanone which can give fermented milk cream and cheese flavor, and significantly enrich amino acid metabolism and carbon metabolism. The fermentation of L. rhamnosus WH. FH-19 increased the contents of L-glutamic acid, taurine, stachyose, erythritol, L-rhamnose, retinol, pantothenic acid and 19 oligopeptides in fermented milk, and endowed fermented milk with good flavor, quality and antioxidant capacity. The results presented that L. rhamnosus WH. FH-19 can increase the content of flavor substances, promote the metabolism of amino acids and carbohydrates in fermented milk, and produce more antioxidant metabolites, which had the potential as a starter of fermented milk.
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MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Huiyu He,Rui Wang,Rongbin Nie,Nan Dong
Trace amounts of pharmaceuticals and personal care products (PPCPs) in aquatic environment poses a non-negligible risk to human health. Here, an environmentally friendly cucurbit[7]uril-mediated magnetic-assisted matrix solid phase dispersion (Q[7]- m -MSPD) extraction method was developed for extracting PPCPs from complex aquatic organisms. The extraction of PPCPs were achieved via the host-guest interaction between Q[7] and targets, significantly reducing the matrix interference. Gold magnetic nanoparticles (AuMNPs) were chelated to Q[7]-target complexes and used for purification and enrichment via magnetic solid-phase extraction (MSPE), effectively replacing the complex operation of sample loading and elution on SPE columns in MSPD. Coupled with high performance liquid chromatography-tandem mass spectrometry, multiple analysis of 14 PPCPs in 3 aquatic plants and an aquatic animal were achieved, with detection limits ranging from 0.0015 to 0.0179 μg/kg, recoveries ranging from 71.06 to 113.6 %, and enrichment factors within 46 to 152. The green chemistry assessment confirmed the environmental friendliness, economic feasibility, and application potential of the Q[7]- m -MSPD, with an AGREE score of 0.63 and a BAGI score of 72.5. By integrating the merits of MSPD and MSPE, the proposed approach exhibited high sensitivity and anti-interference capability, simple operation, and great environmental friendliness. Therefore, the approach provided a green method for simultaneously detecting multiple hazardous residues in complex matrices owing to the broad-spectrum molecular recognition capability of Q[7] , which has a good application prospect in food safety and environmental monitoring.
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危险品化学品经营许可证（带存储）