CHROMATOGRAPHIA
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2018
·Vol. 81
·期 6
·881-889
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IF 1.401
Li Shan,Yang Zhaoguang,Cao Junfei,Qiu Bo,Li Haipu
Abstract The content of metallothionein (MT) in fish can serve as a biomarker for heavy metal contamination in an aquatic environment. In this paper, an improved sample separation and quantification method using cadmium saturation combined with anion exchange high performance liquid chromatography–inductively coupled plasma mass spectrometry (HPLC–ICP-MS) was developed to measure the two major isoforms of MT (MT-I and MT-II) in fish. Replacing sulfur with cadmium as the quantitative element by cadmium saturation reduced the instrumental requirement and analysis cost. In the chromatographic separation, NH 3 –NH 4 Cl buffer was applied as the mobile phase instead of Tris–HCl buffer to prevent carbon deposition on the ICP cone. The chloride concentration was found to be a key factor to the separation of MT-I and MT-II, and the optimum chromatographic condition was 27 mM of NH 3 –NH 4 Cl in isocratic mode, with a pH of 8.6 and a flow rate of 0.8 mL min −1 . The limits of detection were 0.7 μg g −1 for MT-I and 1.0 μg g −1 for MT-II, with recoveries ranging from 96.2 to 104.2% for MT-I and 84.7 to 90.4% for MT-II in different fish tissues. The relative standard deviations were less than 8% for both isoforms. Graphical abstract
研究领域:
环境科学
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分析化学
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毒理学
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DOI
高影响因子
MICROCHIMICA ACTA
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2011
·Vol. 177
·期 1
·23-30
·
IF 2.578
Wu Qiuhua,Liu Min,Ma Xiaoxing,Wang Weina,Wang Chun,Zang Xiaohuan,Wang Zhi
We have developed a highly sensitive microextraction method for the preconcentration of some phthalate esters such as diethyl phthalate, di- n -propylphthalate, di- n -butyl-phthalate, dicyclohexyl-phthalate, and diethyl-hexyl phthalate prior to their determination by HPLC. It is based on a magnetic graphene nanocomposite as an effective adsorbent. The effects of the amount of the extractant composite employed, extraction time, pH values, salt concentration and desorption conditions were investigated. Under the optimum conditions, the enrichment factors range from 1574 to 2880. Response is linear in the concentration range from 0.1 to 50 ng mL −1 . The limits of detection (at S / N = 3) were between 0.01 and 0.04 ng mL −1 . The method was successfully applied to the determination of five phthalate esters in water and beverage samples.
A novel microextraction method was developed by using magnetic graphene nanocomposite as an effective adsorbent for the preconcentration of some trace phthalate esters in water and beverage samples followed by high performance liquid chromatography with ultraviolet detection. The enrichment factors of the method for the compouds were achieved ranging from 1574 to 2880.
研究领域:
分析化学
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环境科学
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DOI
高影响因子
THERAPEUTIC DRUG MONITORING
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2025
·
IF 2.4
Dong Zhonghua,Wang Peng,Cui Xueyan,Liu Jinjuan,Shi Haiyan,Yang Yilei,Xu Jingya,Yi Qiaoyan
Background: Perampanel (PER), a novel antiepileptic drug, exhibits high protein binding. Given the drug's susceptibility to various factors, including drug interactions, and the considerable variability in blood concentrations among individuals, solely measuring the total plasma concentration of PER may not provide comprehensive insights. This study aimed to establish an HPLC-FLD method to quantify both total and free PER in clinical samples. Methods: Analysis of total PER involved a straightforward sample preparation process involving plasma protein precipitation. Plasma samples were ultrafiltered to isolate the free portion of PER. Chromatographic separation was achieved on an InertSustain C18 column at a 1-mL/min flow rate using a gradient of acetonitrile and aqueous sodium acetate buffer at pH 4.4. Results: Calibration curves for total and free PER in plasma exhibited excellent linearity over the concentration ranges of 10–3000 and 0.5–100 ng/mL, respectively. The method was applied to analyze blood samples from patients with epilepsy quantitatively; the total concentration of perampanel in the plasma of the patients was in the range of 90.45–563.39 ng/mL, whereas the free concentration was in the range of 1.82–15.29 ng/mL. The plasma protein binding ratio of perampanel was normally between 97.09% and 99.29% and decreased in cases of hypoproteinemia. Conclusions: The method was rigorously validated for selectivity, accuracy, precision, and stability in accordance with established FDA and EMA guidelines. The developed method enables the rapid and accurate quantification of both total and free PER concentrations in the plasma of patients with epilepsy, offering technical support for its subsequent clinical application.
研究领域:
临床药理学
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分析化学
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神经病学
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DOI
PubMed
高影响因子
PHYTOCHEMICAL ANALYSIS
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2024
·
IF 3
Yangling Li,Ying Su,Yongjuan Liang,Fangchan Li,Ning Lin,Lin Jiang,Qinghua Lin,Qing Chen
Introduction Kidney tea is an essential herbal medicine. It is widely used to treat conditions such as urinary stones, gallstones, and rheumatoid arthritis. There is currently no standardized or widely accepted research strategy for evaluating the quality of kidney tea granules (KTGs) after granulation. Objectives In this study, we aim to establish a comprehensive strategy for evaluating the quality of KTGs produced from different sources of kidney tea. Methods A TLC combined with HPLC method was established to identify the chemical components in KTGs, and HPLC method was used to determine the contents of rosmarinic acid of KTGs. In order to distinguish samples and identify differential components, similarity analysis, hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares discriminant analysis (OPLS-DA) were conducted. Results TLC and HPLC detection confirmed three chemical components of KTGs, which are rosmarinic acid, caffeic acid, and lithospermic acid. HPLC fingerprint analysis revealed a total of seven common peaks in 15 batches of KTGs. Similarity analysis showed that the similarity of all 15 batches of KTGs was greater than 0.969. The peak areas of the seven common peaks were identified by chemical pattern recognition, and the results showed that most of the KTGs from different origins were clustered together, with small differences between them. The PCA and OPLS-DA results showed that two principal components can represent 82.638% of the common peaks of KTGs, among which peak 5 represents rosmarinic acid, which is the main differential biomarker of KTGs from different regions. Quantitative analysis of rosmarinic acid in KTG samples was performed using HPLC fingerprint conditions and the content of rosmarinic acid in 15 batches of KTGs samples was measured to be between 8.01–14.61 mg/g. Conclusion This study combines TLC, HPLC, and chemometrics to establish a stable and reliable method that can quickly and effectively identify the components of KTGs, accurately quantify known components in KTGs, and provide reference for the quality evaluation of KTGs.
研究领域:
中药学
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分析化学
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
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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.
研究领域:
生物化学
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药物筛选
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食品科学
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DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
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2017
·Vol. 40
·期 12
·2528-2540
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IF 2.557
Jinmao You,Kun Dou,Cuihua Song,Guoliang Li,Zhiwei Sun,Shijuan Zhang,Guang Chen,Xianen Zhao,Na Hu,Wu Zhou
A rapid, sensitive, and selective precolumn derivatization method for the simultaneous determination of eight thiophenols using 3-(2-bromoacetamido)- N -(9-ethyl-9 H )-carbazol as a labeling reagent by high-performance liquid chromatography with fluorescence detection has been developed. The labeling reagent reacted with thiophenols at 50°C for 50 min in aqueous acetonitrile in the presence of borate buffer (0.10 mol/L, pH 11.2) to give high yields of thiophenol derivatives. The derivatives were identified by online postcolumn mass spectrometry. The collision-induced dissociation spectra for thiophenol derivatives gave the corresponding specific fragment ions at m/z 251.3, 223.3, 210.9, 195.8, and 181.9. At the same time, derivatives exhibited intense fluorescence with an excitation maximum at λ ex = 276 nm and an emission maximum at λ em = 385 nm. Excellent linear responses were observed for all analytes over the range of 0.033–6.66 μmol/L with correlation coefficients of more than 0.9997. Detection limits were in the range of 0.94–5.77 μg/L with relative standard deviations of less than 4.54%. The feasibility of derivatization allowed the development of a rapid and highly sensitive method for the quantitative analysis of trace levels of thiophenols from some rubber products. The average recoveries ( n = 3) were in the range of 87.21–101.12%.
研究领域:
分析化学
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环境科学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
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2019
·Vol. 34
·期 2
·e4763
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IF 1.748
Qing-ling Qi,Ya-Ming Yu,Cheng Tang
Target biomolecule-immobilized magnetic beads could be used as a powerful tool for screening active compounds present in natural products. Low damage rates of the target proteins, associated with the availability of diverse automated online approaches for analysis, make it a valuable tool for affinity studies. RAW264.7 cells (a kind of murine macrophage cell line) were used in this study. These cellular membranes were immobilized onto the surface of MBs and were used for screening the active compounds of Polygonatum sibiricum. Combining this technique with HPLC led to the identification of an active compound and its biological activity was confirmed. This is the first report establishing the use of RAW264.7 cellular membrane-coated magnetic bead fishing followed by HPLC analysis for screening active compounds from natural products.
研究领域:
药理学
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分析化学
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细胞生物学
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天然产物研究
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
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2020
·
IF 3.594
Baolei Fan,Guoliang Wei,Xiaofeng Gan,Tingting Li,Zengyi Qu,Sheng Xu,Chao Liu,Chunqi Qian
In this study, we reported the various contents of Polygonatum cyrtonema by extracting polysaccharides (PCPs) using steaming and shining procedures, thus providing scientific basis for the processing of Polygonatum cyrtonema and content analysis of polysaccharides. We established the characteristic fingerprint to identify and analyze polysaccharide component changes in distillated and processed Polygonatum cyrtonema by PMP precolumn derivatization and HPLC-MS/MS technology. We also classified two kinds of solutions by comparing the composition difference of 10 polysaccharide components in the samples with principal component and cluster analysis. There was a huge difference between them and seven monosaccharides. Processed PCPs mainly consisted of galactose along with mannose, followed by glucose. Meanwhile, we found that the results of cluster analysis and principal component analysis were the same. The polysaccharide components extracted from processed Polygonatum cyrtonema and distillate were mainly galactose and mannose. The results of cluster analysis and principal component analysis were the same. The distilled liquid can be divided into 5 categories, and the processed dry extract of Polygonatum cyrtonema can be divided into 4 categories. The changing trend of polysaccharide components of Polygonatum cyrtonema and distilled liquid was revealed during the multiple cycles of steaming and sun drying. The similarity and difference of polysaccharide components in the extracted liquid and the distilled liquid of each batch were shown.
研究领域:
中药学
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分析化学
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植物化学
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DOI
高影响因子
MICROCHEMICAL JOURNAL
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2024
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IF 4.9
Linzhou Chen,Jiedan Zhou,Yuesen shi,Fei Xu,Xin Liu,Qingda Huang,Jinjian Zhong,Ke Wu,Dafeng Yang,Huajun Fan,Xiangliang Yang
Collecting exhaled breath aerosols (EBA) as a sample has a great potential to monitoring illicit drug abuse due to advantages of simple, non-invasiveness and unrestricted sampling. However, scarcity of positive samples has cramped development of more efficient techniques for monitoring illicit drug abuse in EBA. In this work, a simulated human exhaled breath aerosol (SHEBA) generating device based on Venturi jet principle was constructed by integrating nebulizing unit and collection unit to prepare positive EBAs. By means of ultra high-performance hyphenated with triple quadrupole tandem mass spectrometry (HPLC-TQ-MS/MS), using caffeine as a target drug, the device parameters were investigated by studying the effects of flow rates of nebulizing and auxiliary gases, drug concentration and etc., the performance was further validated by commonly abused drugs such as amphetamines (AMP, MAMP, MDA and MDMA). Electret material as adsorbent was used to collect SHEBAs generated by the device, achieving HPLC-TQ-MS/MS detection of the captured drugs at 40.0–2000.0 pg/filter. By this way, caffeine content in EBAs from six volunteers was successfully detected in the range of 51.6 ± 6.8–708 ± 51 pg/filter after drinking the caffeinated beverage. These validation experiments proved that SHEBA generating device could not only meet to the requirement of EBA analysis for illicit drug abuse at trace levels, but also provide the correction factors to calibrate the lower detection value caused by incomplete material adsorption.
研究领域:
分析化学
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毒理学
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医学检测
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DOI
高影响因子
FOOD CHEMISTRY
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2025
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IF 9.8
Yupeng Wen,Wendi Huo,Xinyuan Zhang,Yingchun Mu,Huan Liu,Chaoying Zhang,Lu Qiao,Jincheng Li
In this study, we developed a miniaturized semi-automatic purification method based on pressure-filtration purification for sensitive HPLC-MS/MS monitoring of pesticides in aquatic products. For the first time, loofah sponge was demonstrated and utilized as a novel green, low-cost, and effective one-step purification adsorbent for fish sample. The developed method consisted of two main steps: first, target analytes were extracted from fish samples using an acetonitrile-based QuEChERS extraction method. Subsequently, the extract was automatically purified through a pressure-filtration purification column in a centrifuge, followed by HPLC-MS/MS analysis. Under optimized experimental conditions, the method exhibited excellent linearity, with a range of 1.0 to 50.0 μg/kg and a correlation coefficient > 0.99. The detection and quantification limits were 0.5 and 1–2 μg/kg, respectively. Recoveries at spiked levels of 2.0, 5.0 and 30.0 μg/kg ranged from 69.95 to 104.88 %, with intra-day RSDs ranging from 0.58 to 15.01 % and inter-day RSDs ranging from 0.72 % to 14.32 %.
研究领域:
食品科学
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环境科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
Food Chemistry-X
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2023
·
IF 6.1
Yiwei Tang,He Meng,Wenxiu Wang,Yang Song,Shuo Wang,Zhuanying Li,Xianghong Wang,Xuelian Hu
An innovative core–shell magnetic molecularly imprinted polymers, Fe 3 O 4 @SiO 2 @MIPs, was elaborately tailored for specific separation and enrichment of olaquindox (OLA) and its metabolic marker methyl-3-quinoxaline-2carboxylic acid (MQCA). Herein, benefiting from the combination of functionalized magnetic nanoparticles (Fe 3 O 4 @SiO 2 ) and MIPs, Fe 3 O 4 @SiO 2 @MIPs not only possessed favorable magnetic properties and stability, avoiding tedious sample pretreatment process, but also demonstrated exceptional selective recognition ability and adsorption capacity, suppressing influence of coexisting interfering substances. Encouraged by prominent merits, Fe 3 O 4 @SiO 2 @MIPs-based magnetic solid phase extraction with HPLC method was developed, realizing simultaneous measurement of OLA and MQCA. Under optimal conditions, excellent linear ranges of 0–100 μg/L with detection limit of 0.175–0.271 μg/L were obtained. The proposed method was finally utilized for determination of OLA and MQCA in fish muscle and milk samples with satisfactory recoveries (80.56–95.26%) and relative standard deviation below 8.1%, furnishing a reliable and sensitive strategy for enrichment and detection residual veterinary drugs in food samples.
研究领域:
分析化学
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食品安全
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兽药残留检测
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Cai-Fang Liu,Xiao-Yan Ran,Cheng Liu,Yu-lan Zhu,Yan-Rui Lu,Yu-Ping Yang,Bang-Jin Wang,Jun-Hui Zhang,Sheng-Ming Xie,Li-Ming Yuan:
Chiral metal–organic frameworks, an emerging type of chiral porous materials, possess many outstanding characteristics such as high surface area, tunable pore sizes, and good chemical stability. Herein, we prepared a chiral [Zn 2 (D-Cam) 2 (4,4′-bpy)] n @SiO 2 core–shell composite on the SiO 2 -NH 2 microspheres by an in-situ growth method. The prepared [Zn 2 (D-Cam) 2 (4,4′-bpy)] n @SiO 2 -packed column exhibited high-resolution separation of racemic compounds and positional isomers at a low column backpressure (9–12 bar). Twelve pairs of enantiomers including alcohols, amines, epoxides, ketones, and esters were well resolved with sharp peak shapes on the [Zn 2 (D-Cam) 2 (4,4́-bpy)] n @SiO 2 chromatographic column. Compared the separation performance of [Zn 2 (D-Cam) 2 (4,4́-bpy)] n @SiO 2 -packed column and two chromatographic columns (commercial Chiralpak AD-H column and as-prepared SiO 2 -NH 2 column), the [Zn 2 (D-Cam) 2 (4,4′-bpy)] n -packed column and the commercial Chiralpak AD-H column have a good complementarity in chiral separation, and it also offered better separation performance compared to the SiO 2 -NH 2 column for separating positional isomers. The effects of column temperature and analyte mass on the HPLC separation were investigated. Additionally, the [Zn 2 (D-Cam) 2 (4,4́-bpy)] n @SiO 2 packed column has good repeatability and stability for HPLC separation of enantiomers and positional isomers. The relatvive standard deviations (RSDs) for repeated separations of 2,2,2-trifluoro-1-(9-anthryl)ethanol and o , m , p -bromoaniline were less than 0.8 % and 1.2 % for the retention time and peak area, respectively. After continuous use for one month, the RSDs for the retention time and peak area of them were in the range of 1.1–1.3 % and 1.5–1.8 % (inter-day and intra-day, n = 5), respectively. This work also indicates that the chiral MOFs@SiO 2 composites are promising for HPLC separation.
研究领域:
分析化学
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材料科学
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色谱技术
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产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）