JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2014
·
IF 0.638
Juntao Wang,Weina Wang,Qiuhua Wu,Chun Wang,Zhi Wang
A novel graphene-based magnetic nanocomposite (G-Fe3O4) was prepared and used as an effective adsorbent for the preconcentration of some chlorophenols (2-chlorophenol, 3-chlorophenol, 2, 3-dichlorophenol, 3, 4-dichlorophenol, and 2, 4, 6-trichlorophenol) in environmental water samples followed by high performance liquid chromatography-UV detection. Various experimental parameters that could affect the extraction efficiencies, such as the amount of G-Fe3O4, the extraction time, the pH of sample solution and the desorption conditions, have been investigated. Under the optimum conditions, a good linearity existed in the range of 1.0–100.0 ng mL−1 for all the analytes, with the determination coefficients (r2) ranging from 0.9954 to 0.9992. The limits of detection (S/N = 3) of the method were between 0.10 and 0.12 ng mL−1. The relative standard deviations (RSDs) varied from 2.2% to 7.5% (n = 6), and the recoveries of the method for the analytes at spiking levels of 5.0 and 10.0 ng mL−1 were in the range from 85.6% to 107.3%. The method has been successfully applied for the determination of some chlorophenols in environmental water samples.
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CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
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2014
·
IF 0.7
Ren-Dan ZHOU,Lai-Sheng LI,Biao-Ping CHENG,Gui-Zhen NIE,Hong-Fu ZHANG
A 6-azido-β-cyclodextrin was synthesized and derivatized with p -nitrophenyl isocyanate as chiral ligand. Then the ligand was chemically bonded to mesoporous SBA-15 via a ‘Click Chemistry’ reaction of the azido group with alkynyl group. A new p -nitrophenylcarbamoylated β-cyclodextrin bonded SBA-15 chiral stationary phase (NPCSP) for HPLC was thus obtained. The new stationary phase was first used for enantioseparation of propranolol in human plasma under the polar organic solvent mode. The effects of methanol content, concentration of glacial acetic acid/triethylamine in mobile phase and the temperature on the enantioseparation were studied in detail. The optimized chromatographic conditions were as follows: mobile phase was acetonitrile/methanol/glacial acetic acid/triethylamine (90/10/1.25/2.25, V/V ) at 288 K, with a flow rate of 0.5 mL min −1 , an injection volume of 20 μL and detection wavelength at 290 nm. The resolution was 2.04 with a short run time (< 15 min) under the optimal conditions. The content of propranolol in plasma was quantitatively measured by HPLC-MS under selected ion monitoring mode ([M + H] + m/z 260.10) with hydrochlorothiazide as an internal standard. The good linear relationship was observed in the range of 2.5−50 μg L −1 . The detection limits were 1 μg L −1 according to S/N = 3 for both enantiomers. The experimental results showed that the chiral stationary phase exhibited excellent chiral separation ability to propranolol. The analytical method for propranolol enantiomers was sensitive, accurate, simple and fast, which was can be for the determination of propranolol in plasma and related pharmacokinetic studies.
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Food Analytical Methods
·
2016
·Vol. 9
·期 12
·3298-3309
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IF 2.167
Wang Chao,Zhang Chen-Xia,Shao Chun-Fu,Li Chang-Wen,Liu Shun-Hang,Peng Xiao-Pei,Xu Yong-Quan
A simple and efficient fingerprint analysis method was developed and validated for the quality consistency control and authentication of Deepure instant pu-erh tea within different manufacturers using high-performance liquid chromatography (HPLC) coupled with chemometrics. To compare the HPLC fingerprint chromatograms between batches, varieties and manufacturers, the correlation coefficients of similarities of 60 samples and the relative peak areas of 11 characteristic compounds were calculated. Different pattern recognition procedures, including hierarchical cluster analysis, principal component analysis and partial least squares discriminant analysis, were then applied to classify the instant pu-erh tea samples according to their variety and manufacturer. Results showed that the developed method has potential application for the quality consistency evaluation and discrimination of instant pu-erh tea samples from similar products.
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MICROPOROUS AND MESOPOROUS MATERIALS
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2017
·
IF 3.615
Yajun Du,Lingping Cheng,Long Chen,Yunchao He,Yaling Wu,Shanshan He,Yanxiong Ke
Sub-2 μm large-pore monodispersed mesoporous silica spheres (MMSS) were synthesized by using mixed non-ionic surfactants of dodecylamine (DDA) and dodecylamine polyoxyethylene ether (AC1210) as templates through an alkali-catalyzed silica sol–gel technique combined with the template method. Methanol-H 2 O volume ratio on morphology was researched in detail. In addition, by using hydrothermal treatment , the average pore size of MMSS could be enlarged to 11 nm from 4.4 nm. The mesoporous silica particles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), laser particle size analyzer, X-ray diffraction, N 2 physisorption technique. The synthesized sub-2 μm monodispersed mesoporous silica microspheres were successfully functionalized by dimethyloctadecylchlorosilane and used as a packing material in high performance liquid chromatography (HPLC).
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INTERNATIONAL JOURNAL OF FOOD SCIENCE AND TECHNOLOGY
·
2024
·Vol. 59
·期 4
·2689-2696
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IF 2.6
Jin-Yu Li,Yun-Jiao Ma,Feng Xiao,Xian-Bing Xu
Summary On-site sample preparation has the advantage of combining sampling and sample preparation into a single step, thereby minimising sources of error, and eliminating the risk of analyte instability. Bubble-driven solid-phase microextraction (BD-SPME) was first proposed as an on-site pretreatment method. Oyster sauce underwent on-site pretreatment to measure potassium sorbate levels via high-performance liquid chromatography with a diode array detector (HPLC-DAD), obviating the need for stirrers. The high sensitivity of the HPLC determination of potassium sorbate was obtained using BD-SPME pretreatment with a limit of detection (LOD) of 0.03 mg L −1 and a limit of quantification (LOQ) of 0.10 mg L −1 . The refined technique displayed remarkable linearity from 0.10 to 30.00 mg L −1 , boasting a coefficient of determination R 2 ≥ 0.998. In addition, the recoveries of potassium sorbate in oyster sauce using the method were in the range of 90.8–101.4%. Evidently, BD-SPME in combination with HPLC-DAD is a sensitive and promising analysis for on-site pretreatment.
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PHYTOCHEMICAL ANALYSIS
·
2017
·Vol. 28
·期 5
·424-432
·
IF 2.292
Binjun Yan,Xue Bai,Yunjie Sheng,Fanzhu Li
Introduction On account of the complicated compositions of the products like traditional Chinese medicines (TCMs) and functional foods, it is a common practice to determine different sets of analytes in the same product for different purposes. Objective To efficiently develop the corresponding HPLC methods, a statistical model based analytical method adjustment (SMB-AMA) strategy was proposed. Methods In this strategy, the HPLC data acquired with design of experiments methodology were efficiently utilised to build the retention models for all the analytes and interferences shown in the chromatograms with multivariate statistical modelling methods. According to the set of analytes under research, Monte-Carlo simulations were conducted based on these retention models to estimate the probability of achieving adequate separations between all the analytes and their interferences. Then the analytical parameters were mathematically optimised to the point giving a high value of this probability to compose a robust HPLC method. Radix Angelica Sinensis (RAS) and its TCM formula with Folium Epimedii (FE) were taken as the complicated samples for case studies. Results The retention models for the compounds in RAS and FE were built independently with correlation coefficients all above 0.9799. The analytical parameters were tactfully adjusted to adapt to six cases of different sets of analytes and different sample matrices. In the validation experiments using the adjusted analytical parameters, satisfactory separations were acquired. Conclusion The results demonstrated that the SMB-AMA strategy was able to develop HPLC methods rationally and rapidly in the adaption of different sets of analytes. Copyright © 2017 John Wiley & Sons, Ltd.
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MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Zi-Yu Li,Jia-Hui Zhu,Sheng-Nan Lv,Jie Zhao,Xiao-Shuai Yang,Yu-Shen Liu,Zhen-Hua Hu,Ting Cheng,Yan-Xin Chen,Lu-Liang Wang
Diclofenac (DCF), as fifth veterinary drugs, is a popular non-steroidal anti-inflammatory drug, widely applied in pain relief and anti-inflammatory of humans and animals, and endanger human health and food safety. Developing the effective technology for the removal or trace detection of DCF is urgent. Therefore, rational design and preparing advanced and selective adsorbent is extremely significant. Herein, a novel sulfonic acid (Sa) functionalized covalent organic frameworks (Fe 3 O 4 @TpbDva-Sa) were designed and prepared to enrich and determine trace DCF in milks with the aid of high performance liquid chromatography (HPLC). Fe 3 O 4 @TpbDva-Sa adsorbent was well characterized. The parameters of magnetic solid phase extraction (MSPE), adsorption kinetic and isotherm were evaluated in detail. Furthermore, adsorption mechanism of Fe 3 O 4 @TpbDva-Sa for DCF was investigated. The developed Fe 3 O 4 @TpbDva-Sa-MSPE-HPLC method was validated and employed to detect trace DCF in food samples. The established method displayed low dosage (2 mg), good linearity (8 × 10 -4 -10 μg mL −1 ), low limit of detection (2.4 × 10 -4 μg L -1 ), large adsorption capacity (98.03 mg g −1 ), good reusability and satisfactory recoveries (87–98 %). This work reported the novel magnetci sulfonic acid-based covalent organic frameworks for MSPE of DCF. The results revealed the great potency of Fe 3 O 4 @TpbDva-Sa for enriching the residues of veterinary drug in complex matrix and uncovered the prospects of functional covalent organic frameworks in sample pretreatment.
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MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Qi Zhou,Lihong Wang,Canping Pan,Congcong Yu,Jin Hua,Tao Lan
Considering the matrix characteristics of honeysuckle and chrysanthemum, a comprehensive and systematic extraction and purification processes study for pesticide residue analysis in these two Traditional Chinese Medicine (TCM) were conducted based on a nanomaterial-modified QuEChERS method. For honeysuckle, a combination of 60 mg FeN-MWCNTs and 60 mg PSA provided the best purification effect. For chrysanthemum, 70 mg GCB and 30 mg PSA achieved the optimal results. Our initial exploration into the purification mechanism of the nanomaterials revealed that micropores and smaller mesopores in the adsorbents play a crucial role, while amino groups primarily govern the adsorption process, with matrix impurities adhering to the surface of the nano-adsorbents. The limit of quantification (LOQ) for honeysuckle in this method ranged from 0.12 to 18.86 µg/kg, with recovery rates between 60.1 % and 128.6 %, and relative standard deviations (RSD) less than 12 %. For chrysanthemum, the LOQ was between 0.10 and 8.56 µg/kg, and the recovery rates for 27 pesticides were in the range of 61.6 % to 118.9 %. Applying this method, 105 honeysuckle and 111 chrysanthemum market samples were analyzed, detecting five pesticides in 18 honeysuckle and 12 chrysanthemum samples respectively. This study offers a targeted strategy for the development of analytical methods for trace substances in complex matrices.
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ACS Omega
·
2024
·
IF 3.7
Jianwu Lu,Yinfei Shi,Xiaoxia Ye,Shun Yuan,Xiaolong Yang,Xun Sun,Taizhi Wu
The primary limitations of the quantitative analysis of thermally labile halogenated compounds by traditional gas chromatography (GC) are the inadequacy of identifying the insufficiently volatile impurity (often with a high boiling point) and the difficulty in obtaining a standard substance with a reliable standardized assay. Taking the 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one (DMDO-Cl, 1) as an example, we reported a triphenylmethanamino-derivatization method to overcome the challenges of the assay determination of such species. During the quantification of 1, the presence of GC-undetectable polymeric impurity 10 poses a critical challenge in assessing the material quality. Moreover, the standard substance of 1 is not available on the market due to its inherent instability during storage and handling, further complicating the quantitative analysis. In this work, a precolumn HPLC-UV derivatization method based on triphenylmethanamino-alkylation was developed to quantitatively analyze 1. The resulting derivative 2 exhibits excellent crystallinity and superior physical and chemical stability and possesses effective chromophores for UV detection. The conversion from analyte 1 to derivative 2 demonstrates desirable reactivity and purity, facilitating quantitative analysis using the external standard method. The chemical derivatization-chromatographic detection method was optimized and validated, demonstrating its high specificity, good linearity, precision, accuracy, and stability. This method offers a valuable alternative to the general quantitative NMR (qNMR) detection technique, which exhibits reduced specificity in the presence of increased levels of impurities in compound 1.
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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY
·
2017
·Vol. 32
·期 6
·1186-1195
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IF 3.379
Shan Li,Beibei Chen,Man He,Bin Hu
Protein phosphorylation analysis is important for understanding cell regulations. Mass spectrometry (MS) is a powerful technique for peptide phosphorylation analysis. However, quantification of low abundance phosphoproteins in a complex mixture of proteins is still a challenge. Here we report the development of hollow fiber (HF) supported TiO2 monolithic microextraction combined with capillary high performance liquid chromatography (capHPLC)-inductively coupled plasma-collision reaction cell (ICP-CRC)-MS for the absolute quantification of phosphopeptides. The membrane pores (∼200 nm) of the HF effectively carry more TiO2 on its surface to enhance the adherence of the TiO2 monolith with the HF. By using β-casein as a model phosphorylated protein, we optimized the HF-supported TiO2 monolithic microextraction towards phosphopeptides. Under the optimal conditions, a 100-fold enrichment factor was obtained and the monoliths can be reused 40 times. By monitoring 31P16O with O2 as a reaction gas in the CRC, polyatomic mass interference at m/z 31 is avoided and a low detection limit (2.9 nM) of phosphorus is achieved. The method of HF-supported TiO2 monolithic microextraction-capHPLC-ICP-MS provided the detection limit for phosphopeptides at the nM level. The proposed method was applied to the quantification of phosphopeptides in milk and milk powder samples.
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BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 4
·e70000
·
IF 1.7
Shuyan Xue,Feichao Song,Na Wei,Yuxuan Liu,Muchun Liu,Xi Huang,Yumeng Zhang,Yang Liu,Huiqin Hao,Junfeng Zhang
We aim to establish the fingerprint profile of Er Miao San (EMS) that aims to accurately evaluate the quality of EMS samples and to identify quality markers for different batches of EMS and explore its related targets and pathways for the treatment of rheumatoid arthritis. HPLC was employed with an Agilent C18 column. Cluster analysis and principal component analysis were conducted by using SPSS and SIMCA software. Network pharmacology techniques were utilized to explore the potential targets and pathways of EMS in the treatment of rheumatoid arthritis. The HPLC fingerprint profile of EMS was established, featuring a total of 15 common peaks, among which nine were identified. The 10 batches of medicinal materials could be clustered into three categories. With VIP > 1 as the criterion, four index differential components were screened out. These intersections were imported into the STRING database and Cytoscape software, resulting in 228 intersection targets. GO and KEGG enrichment analyses were performed on the related targets and pathways. The established method can effectively analyze the quality differences of EMS from different origins. The screened targets and pathways are of great significance for analyzing the differences in the treatment of rheumatoid arthritis by different batches of EMS.
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Food Analytical Methods
·
2022
·Vol. 15
·期 9
·2479-2486
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IF 3.498
Zhang Shengnan,Li Zhibo,Qi Yanxia,Yu Pei,Zhao Qiancheng
The determination of 2-acetyl-1-pyrroline (2-AP), which is an important flavour compound of crustaceans and has a low odour threshold of 0.05 μg/L in water, is still a challenge due to the instability and trace levels of 2-AP in food samples. In this study, 2-AP was trapped by o-phenylenediamine and subsequently purified by the dispersive solid-phase extraction and dispersive liquid–liquid microextraction (DSPE-DLLME) methods for HPLC–UV analysis. The developed method was simple, fast and sensitive for the determination of 2-AP in shrimp. Under the optimized DSPE-DLLME conditions, the developed method exhibited excellent linearity ( R 2 = 0.996) and a low limit of detection (LOD, 1.77 μg/kg) and limit of quantitation (LOQ, 5.33 μg/kg). The recoveries of 2-AP in shrimp ranged from 86.3 to 101.6%. In addition, the developed method was applied to detect 2-AP levels in baked shrimp (ranging from 5.6 to 12.6 μg/kg), indicating that the formation of 2-AP could be observed in thermally treated shrimp depending on heating temperature and time. In summary, the developed method has potential application for the trace determination of 2-AP in shrimp due to its convenience and high sensitivity.
研究领域:
食品科学
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分析化学
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危险品化学品经营许可证（带存储）