ANALYTICAL CHEMISTRY
·
2025
·
IF 6.7
Lu huang,Hong Jiang,Bin Li,Lanying Chen,Tongtong Yang,Jiang Wang,Huanwen Chen
An online reactive internal extraction electrospray ionization (iEESI) method was developed for the rapid determination of organic and inorganic speciation information for selenium in poultry tissue samples without complex sample pretreatment. The addition of citric acid as a reducing agent to the internal extraction solvent of methanol/acetic acid (99:1, V/V) for iEESI resulted in the reduction of selenate in the sample to selenite, accompanied by the production of malic acid as an oxidation product. The quantitative analysis of selenate was conducted by using malic acid. By addition of o-phenylenediamine (OPD) to the extractant, inorganic selenium including selenite and selenite reduced from selenate was immediately extracted and converted into 1,3-dihydro-2,1,3-benzoselenadiazole after an in situ reaction. The methanol in the reagent extracted organic selenium compounds from the samples, enabling a rapid quantitative analysis of organic and inorganic selenium in chicken tissue. The concentrations of selenomethionine (SeMet), l-selenocystine (SeCys(2)), selenite, and selenate in different tissue samples were examined, showing strong linearity in the range of 1.00–100.00 μg/kg with the limit of detection (LOD) ranging from 0.36 to 0.84 μg/kg. The results were validated by two conventional methods with an accuracy of 84.2–107.6%. The quantitative analysis of three chicken visceral samples revealed that the highest concentration of organic selenium was present in chicken livers, while the highest concentration of inorganic selenium was observed in gizzards. The findings may provide a reliable method for studying selenium metabolism pathways in organisms.
研究领域:
分析化学
·
营养学
·
生物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2025
·
IF 3.8
Sha Dandan,Yuan Minghui,Zhang Lin,Li Hongli
Insulin bound with ligand molecules can improve its bioavailability in oral formulations. In this work, the interactions between insulin and bile acids of taurocholic acid (TCA) and glycocholic acid (GCA) are characterized using different mass spectrometry (MS) methods. Electrospray (ESI)–MS analysis revealed that GCA and TCA could interact with insulin individually or together through non-covalent bonds, and the products included mGCA-insulin, nTCA-insulin, and mGCA-nTCA-insulin complexes. Their binding stoichiometry, relative intensity ratio ( IRa ), and binding affinity were determined. ESI–MS/MS data and the calculated association constants both suggest that TCA has stronger affinity to insulin than GCA. The mixtures of various insulin, GCA, and TCA complexes with different charge states were separated, and distinct trend lines were observed using ion mobility mass spectrometry (IMMS). Moreover, liposomes containing insulin and GCA and/or TCA were prepared, and directly characterized using ESI–MS, and the interaction products of insulin with GCA and TCA were found in the liposome formulation. AutoDock was used to simulate molecular binding and select binding sites between insulin and GCA or TCA to explore the interaction mechanisms. The findings in this work could help understand the mechanism of action of insulin protection with bile acids in the body. Graphical
研究领域:
药学
·
分析化学
·
生物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Mingying Ma,Tianhao Wu,Zhian Hu,Gongwei Sun,Sichun Zhang
High-throughput sample preparation is important in clinical mass spectrometry (MS) analysis. In this work, we developed a method by coupling Nano-ESI-MS with magnetic SPE using a MOF material, Fe 3 O 4 @UiO-66, as sorbent for simultaneous determination of testosterone (T) and androstenedione (4-AD) in serum samples. The proposed method presented good linearity in the range of 0.1–5 μg/L and the recoveries of serum samples were 90.7%-110.0% and 101.7%-108.7% for T and 4-AD, respectively. The results indicated that the Fe 3 O 4 @UiO-66 is an ideal sorbent for androgens extraction and the method is reliable for high-throughput quantitation of T and 4-AD in clinical applications.
研究领域:
分析化学
·
临床医学
✓ 已验证
DOI
高影响因子
JOURNAL OF MASS SPECTROMETRY
·
2017
·Vol. 52
·期 7
·411-416
·
IF 2.381
L. Wang,Y. Wang,Y. Chai,Y. Kang,C. Sun,S. Zeng
A facile method based on electrospray mass spectrometry was established and validated for the differentiation of enantiomeric tadalafil isomers without using chiral chromatographic separation. The enantiomers were coupled with a chiral selector to form diastereomeric complex ions. Nickel–tadalafil complexes, [Ni II (tadalafil)( l -Trp)-H] + , produced a characteristic fragment ion at m / z 524 by loss of 1-methyl-1,6-dihydropyrazine-2,5-dione via collision-induced dissociation. The relative abundance of this fragment ion to the precursor contributed to differentiate tadalafil enantiomers, and energy-resolved product-ion spectra were applied to determine the molar composition of tadalafil in the mixture ( R , R and S , S ) as well. In addition, the other two forms of stereomeric isomers of tadalafil ( R , S and S , R ) could be also distinguished and analyzed by this method. The method was validated in different types of mass spectrometers (AB quadrupole time-of-flight and Bruker ion trap) and also verified by a chiral high-performance liquid chromatography coupled with quadrupole time-of-flight. The chiral determination of tadalafil using MS method proved to be rapid (1-min run time for each sample) and to have the same accuracy and precision comparable to chiral liquid chromatography mass spectrometry methods. This method provides an alternative to commonly used chromatographic technique for chiral determination and is particularly useful in rapid screening in enantioselective synthesis and enantiomeric impurity detection in pharmaceutical industry. Copyright © 2017 John Wiley & Sons, Ltd.
研究领域:
分析化学
·
药物化学
·
质谱分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2024
·
IF 4
Shuai Zhuang,Huihui Ming,Wenjie Yu,Liping Luo
Royal jelly (RJ) is a highly perishable food during storage. However, the quality of RJ is hard to evaluate due to its complex and variable compositions. Nanoliter electrospray ionization mass spectrometry (nano-ESI-MS) is an emerging direct mass spectrometry method suitable for rapid analysis of complex food components and food quality. In this study, we investigated the freshness and metabolite changes of RJ stored at 4 °C and 25 °C using nano-ESI-MS and verified the results with UPLC-Q/TOF-MS. The nano-ESI-MS identified 20 compounds and quantified 9 metabolites with high stability and reproducibility. Multivariate analysis of the nano-ESI-MS data distinguished RJ of different freshness and suggested 45–60 and 7 days as the freshness threshold of RJ stored at 4 °C and 25 °C, respectively. The multivariate analysis of UPLC-Q/TOF-MS data output similar results to that of nano-ESI-MS. The relative abundance changes of metabolites identified by UPLC-Q/TOF-MS were approximately consistent with the quantification results of nano-ESI-MS, indicating the reliability of nano-ESI-MS in monitoring RJ freshness. This study proved the potential of nano-ESI-MS as a rapid method for monitoring RJ freshness and thus promoted the quality control of RJ during production.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
TALANTA
·
2017
·
IF 4.162
Jiang Wang,Xiao-Xiao Jiang,Wei Zhao,Jun Hu,Qi-Yuan Guan,Jing-Juan Xu,Hong-Yuan Chen
The direct separation and analysis of chiral drugs in the complex matrix systems are meaningful and challenging. As the most common broad-spectrum antibiotic, levofloxacin has a strong antibacterial ability, but its enantiomer , dextrofloxacin can cause serious harm to human health. In this work, we reported a rapid on-line extraction/ionization device coupled with Electrospray Mass Spectrometry (ESI-MS) for chiral analysis of ofloxacin enantiomers in complex matrix of milk. Since ofloxacin is difficult to dissolve in water and most organic solvents, the procedure of separating ofloxacin in complex system is often complicated. Using the homemade apparatus, the sample pretreatment process was greatly simplified. Milk sample was directly injected and chiral ofloxacin in the sample was extracted at PTFE membrane for further ionization. It took less than 10 s to finish all the procedures including sampling, extraction, reagents mixing, ionization and mass analysis. Utilizing reaction thermodynamics method , trimeric cluster ion [Ni ΙΙ (ref) 2 Ofloxacin-H] + was formed and collisionally dissociated to get chiral resolution of levofloxacin and dextrofloxacin due to the different relative stabilities of the two diastereomeric clusters produced through the dissociation of Ni ΙΙ bound trimeric clusters. With the proposed method, qualitative and quantitative chiral analysis of ofloxacin in milk was successfully achieved in a simple and fast way.
研究领域:
分析化学
·
药物分析
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2019
·
IF 4.916
Pengfei Yang,Xinyi Wang,Zhenggui Gu,Huihui Li,David D.Y. Chen,Xiaodi Yang
A 15-mer thrombin-binding aptamer (TBA) was discovered with specificity for thrombin. It forms a unique G-quadruplex (G4), which is postulated to be the molecular basis for its binding specificity. Many analytical methods make use of affinity binding between the thrombin and TBA as they form a very stable complex. We develop a strategy to stabilize TBA/G4's structure by introducing G4-interactive molecules, which may enhance its ability to recognize the target. Herein, a fast screening ESI-MS assay was employed to determine potential binding of natural products molecules with the TBA/G4 complex. The experimental results showed that four investigated natural alkaloids had apparent binding affinities. One of them, jatrorrhizine (L1), has been shown to bind strongly to the TBA/G4 mainly in 1:2 M ratio. Once the working conditions were established, the interaction of the jatrorrhizine with the TBA/G4 was explored using a combination of ESI-MS and spectroscopic techniques. Ligand-induced effects on TBA/G4 structure and its stability were examined by means of circular dichroism (CD). Jatrorrhizine inducing the G4 formation seems also to be the more effective in terms of thermal stabilization under the experimental conditions used. Both results of UV and fluorescence experiments undoubtedly showed a good binding affinity with the binding constant around 10 5 L mol −1 . The stacking interactions of jatrorrhizine with the G-tetrads in TBA/G4 were further confirmed by competition experiment. ESI-MS was carried out to determine the coexistence of 1:1 and 1:2 complexes in TBA/G4-L1 system, and showed a dynamical shift from 1:1 to 1:2 complex in minutes.
研究领域:
生物化学
·
分子生物学
·
药物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2022
·
IF 5.304
Xinying Gong,Linyan Xu,Xiaoxue Kou,Juan Zheng,Yixin Kuang,Suxin Zhou,Siming Huang,Yu Zheng,Wei Ke,Gousheng Chen,Gangfeng Ouyang
The ubiquitous occurrence of perfluoroalkyl acids (PFAAs) in environmental water has drawn much attention due to their high persistence and bioavailability. However, it is difficult for the traditional adsorbents to extract PFAAs because of their unique hydrophobic and oleophobic properties. In this study, an amino-functionalized ZIF-8 (NH 2 -ZIF-8) was fabricated and used as the coating materials of the solid-phase microextraction fiber for the determination of PFAAs in water samples. The introduction of the amino group improved the extraction performance of PFAAs via electrostatic interaction and hydrogen bond, which exhibited better extraction efficiencies than those of ZIF-8 coated fiber and commercial fibers. The extraction efficiencies of PFAAs decreased with the increase of pH values, indicating that electrostatic interaction between the carboxylic acid group of PFAAs and the amino group of NH 2 -ZIF-8 played a dominating role in enrichment. The fabricated fiber coupled with high-performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS) was used for the detection of PFAAs in water samples, with a wide linear range (1–5000 ng L −1 ), low limits of detection (0.15–0.75 ng L −1 ), and good repeatability and reproducibility (1.9%-15.5%). The established method has been successfully applied in environmental water analysis, which provides a practical method for the determination of PFAAs in a convenient manner.
研究领域:
分析化学
·
环境科学
✓ 已验证
产品关联
DOI
高影响因子
Journal of Zhejiang University-SCIENCE B
·
2013
·Vol. 14
·期 7
·604-614
·
IF 1.108
Wang Shu-fang,Leng Jing,Xu Yi-min,Feng Mei-ling
Xiongdankaiming tablet (XDKMT), a well-known compound in traditional Chinese medicine, is widely used for the treatment of acute iridocyclitis and primary open-angle glaucoma. In this paper, accurate and reliable methods were developed for the identification of 20 constituents using high-performance liquid chromatography with photodiode array and electron spray ionization-mass spectrometry (HPLC-PDA/ESI-MS n ), and determination of nine of the constituents (chlorogenic acid, gentiopicroside, isochlorogenic acid B, diosmetin-7- O -β- d -glucopyranoside, apigenin, diosmetin, tauroursodeoxycholic acid, acacetin, and taurochenodeoxycholic acid) was developed using HPLC with ultraviolet absorption detector and evaporative light scattering detector (HPLC-UV/ELSD) for the first time. The best results were obtained on a Zorbax SB-C18 column with gradient elution using water (0.1% formic acid) (A) and methanol (0.1% formic acid) (B) at a flow rate of 0.7 ml/min. Tauroursodeoxycholic acid and taurochenodeoxycholic acid, owing to their low UV absorption, were detected by ELSD. The other seven compounds were analyzed by HPLC-UV with variable wavelengths. The calibration curves of all nine constituents showed good linear regression ( R
2 >0.9996) within the linearity ranges. The limits of detection and quantification were in the ranges of 0.0460–9.90 μg/ml and 0.115–24.8 μg/ml, respectively. The accuracy, in terms of recovery, varied from 95.3% to 104.9% with relative standard deviations (RSDs) less than 4.4%. Precision (with the intra- and inter-day variations less than 4.4%) was also suitable for its intended use. The developed method was successfully applied for the analysis of major components in XDKMT, which provides an appropriate method for the quality control of XDKMT.
研究领域:
中药学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
ATMOSPHERIC ENVIRONMENT
·
2017
·
IF 3.629
Rui Li,Xinfeng Wang,Rongrong Gu,Chunying Lu,Fanping Zhu,Likun Xue,Huijun Xie,Lin Du,Jianmin Chen,Wenxing Wang
Particulate biogenic organic nitrates (PBONs) are important components of secondary organic aerosols and play an important role in the tropospheric atmosphere chemistry. However, the concentrations and the chemistry of PBONs remain poorly understood due to the lack of accurate measurement techniques on specific organic nitrates. In this study, ultra high performance liquid chromatography/electrospray mass spectrometry was applied in detection of individual PBONs in ambient atmosphere. Total five kinds of PBONs were identified in PM 2.5 samples collected in urban Ji'nan in spring according to characteristic fragments of NO 2 , NO 3 , HNO 3 , CO 2 , and H 2 O, including monoterpene hydroxyl nitrate (MW = 215, MHN215), pinene keto nitrate (MW = 229, PKN229), limonene di-keto nitrate (MW = 247, LDKN247), oleic acid keto nitrate (MW = 359, OAKN359), and oleic acid hydroxyl nitrate (MW = 361, OAHN361). Among them, three kinds of PBONs originated from biogenic volatile organic compounds of pinene and limonene and two kinds of PBONs came from chemical conversion of oleic acid. The concentrations of these PBONs were roughly quantified with surrogate standards of (1R,2R,5R)-(+)-2-hydroxy-3-pinanone and ricinoleic acid. The average concentrations of MHN215, PKN229, LDKN247, OAKN359, and OAHN361 were 111.6 ± 23.0, 93.1 ± 49.6, 55.3 ± 7.4, 23.4 ± 14.5, 36.8 ± 18.3 ng m −3 , respectively. The total concentration of these PBONs was 325.4 ± 116.7 ng m −3 , contributing to 1.64 ± 0.34‰ of PM 2.5 .
研究领域:
环境科学
·
分析化学
✓ 已验证
DOI
高影响因子
ANALYTICAL CHEMISTRY
·
2025
·
IF 6.7
Meng Zhang,Yanxiao Jiang,Qiong Wu,Hong Zhang,Kai Yu,Guangfeng Kan,Daqian Song,Jie Jiang
The direct mass spectrometric analysis of complex biological samples is often hindered by matrix interference and the need for extensive sample preparation. In this study, an online electroextraction method based on nano-electrospray mass spectrometry (OEE–nESI–MS) was proposed for the high-sensitivity and rapid analysis of urine samples. Compared with other methods, OEE–nESI–MS requires only 5 μL of sample and 35 μL of extraction solvent to achieve the migration and simultaneous ionization of the target from the sample solution to the extraction solvent in the nano tip, and online extraction and simultaneous analysis can be achieved within 8 min, while maintaining comparable sensitivity to other detection methods. The OEE–nESI–MS showed good linearity (R2 > 0.995) in the range of 1–600 ng mL–1 for the five catecholamines (CAs) in urine, with detection limits as low as 0.39–0.89 ng mL–1 with recoveries of 91.9–104.9% (RSD ≤ 8.9%). Exploration of the OEE–nESI mechanism emphasized the electric field applied as a key factor facilitating online electroextraction. The OEE–nESI–MS was successfully applied to the analysis of five CAs in real urine samples. This advancement provides a very simplified solution for the online rapid, highly sensitive, and quantitative determination of complex samples.
研究领域:
分析化学
·
质谱分析
·
生物分析化学
·
临床诊断
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF MOLECULAR LIQUIDS
·
2023
·
IF 6
Daiyun Gu,Jianru Li,Cunying Xu,Shuxian Wang,Guilin Xiang,Wenkang Chen,Qibo Zhang,Yixin Hua,Yan Li
The influence of existing form of different zinc compounds on the electrochemical behavior of zinc was investigated in choline chloride-urea (ChCl-urea) deep eutectic solvent (DES). Raman and ESI-MS analyses indicate that complexes [ZnCl 4 ] − , [Zn(H 2 O)Cl 3 ] − and [ZnO⋅urea⋅Cl] − are presented in the ChCl-urea DES containing ZnCl 4 , ZnSO 4 ⋅7H 2 O and ZnO, respectively. The zinc compounds were found to vary reduction overpotential of Zn(II) ions in the order ZnO > ZnSO 4 ⋅7H 2 O > ZnCl 4 , while their reduction and diffusion rate in a sequence ZnSO 4 ⋅7H 2 O > ZnCl 4 > ZnO. This may be due to the formation of various Zn(II) complexes and oligomers. The chronoamperometric transient analysis shows that Zn electrodeposition in ChCl-urea DES with ZnCl 2 or ZnO as a precursor follows instantaneous nucleation mode, while ZnSO 4 ⋅7H 2 O is changed to a more progressive one. Besides, the zinc compounds can alter the rate of nucleation, influencing the morphology of zinc deposits. The ChCl-urea DES containing ZnSO 4 ⋅7H 2 O or ZnO is conducive to electrodeposition of a smooth and dense zinc coating. The XRD analysis of the deposits displays that part of the deposited zinc is able to alloy with copper substrate to form the Zn-Cu surface alloy, and the amount of the alloy depends on zinc compound. These findings promise a cheap and simple route for production of Zn coating directly form Zn secondary resources.
研究领域:
电化学
·
材料科学
·
分析化学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）