Analytical Methods
·
2024
·Vol. 16
·期 16
·2472-2477
·
IF 2.7
Chenhao Zhao,Xingdan Wang,Jing Wu,Yeli Hu,Qiwei Zhang,Qi Zheng
Sialic acids are a family of monosaccharides that share a nine-carbon backbone and a carboxyl group. A recent derivatization method based on 3-nitrophenylhydrazine (3-NPH) provides a mild chemical labeling technique for biomolecules containing carbonyl or carboxyl groups. In this study, we utilized 3-NPH to label sialic acids via a two-step derivatization process. The derivatized species can produce a common reporter ion corresponding to C1–C3 with two labels, and a fragment differentiating between Neu5Ac, Neu5Gc, and KDN. This method is compatible with O-acetylated sialic acids and provides high sensitivity to Neu5Gc and KDN, and since the utilization of dual labeling significantly enhances the hydrophobicity of derivatives, it can effectively mitigate matrix effects when combined with parallel reaction monitoring technology. Negative-ion tandem mass spectrometry (MS/MS) analysis reveals a distinctive fragmentation profile for the 4-O-acetylated species, while the other sialic acids yield similar MS/MS spectra with a high abundance of reporter ions. Using the reporter ion as a transition, this analytical strategy is effective for analyzing complex biological samples. For example, it was successfully employed to quantify sialic acids in the intestinal tissues of several carp species, demonstrating its potential in sialylation research.
研究领域:
分析化学
·
糖生物学
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DOI
PubMed
高影响因子
EUROPEAN POLYMER JOURNAL
·
2021
·
IF 4.598
Zhiyuan Meng,Jie Yin,Fei Zhao,Mingxin Li,Yan Zhang,Yueyin Liang,Zhonglong Wang,Yiqin Yang
2,4-Dinitrophenylhydrazine (DNPH) is widely present in the ecological environment and has great harmful effects on humans, so it is necessary to detect DNPH in environmental samples. Chitosan, the second abundant renewable biological material in natural, has the advantages of wide sources, good biodegradability and good biocompatibility. Naphthalimide is a kind of classical fluorophore and has widely applications in fluorescent probe field. In this paper, a new fluorescent probe CTS-NA-OAc for DNPH detection was developed, which was constructed by using chitosan as skeleton and naphthalimide as the fluorophore. This probe displayed a highly specific “turn-off” fluorescence response toward DNPH, accompanied by the fluorescence color change from green to colorless. Its detection limit for DNPH was calculated to be 4.9 × 10 −7 M and much lower than that of the corresponding model compound NA-OAc . The interference experiments showed that other competing analytes have no influence on the detection of DNPH in a complex environment. In addition, the coordination mechanism of CTS-NA-OAc with DNPH was investigated by 1 H NMR titration and DFT calculations. Inspired by the above prominent performances, the probe CTS-NA-OAc was successfully applied to the detection of DNPH in real water and soil samples.
研究领域:
环境科学
·
生物化学
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DOI
高影响因子
NEW JOURNAL OF CHEMISTRY
·
2022
·Vol. 46
·期 22
·10777-10786
·
IF 3.925
Xiaoxia Yu,Jianye Pei,Lihua Bi
To develop an excellent electrochemical sensor for the detection of 2,4-dinitrophenylhydrazine (2,4-DNPH), which has become a primary organic pollutant in the environment and is greatly poisonous, four polyoxometalates (POMs) with different structures (H3PW12O40: PW12, K6P2W18O62: P2W18, K12.5Nal.5[NaP5W30O110]·15H2O: P5W30, K28Li5H7P8W48·92H2O: P8W48) were chosen to investigate their sensing performance in solution and composite films towards the detection of 2,4-DNPH. The results indicated that the composite film containing P8W48 exhibited the best performance among the four POMs. The study focused on the effect of the layer number and solution pH on the sensing performance of the composite film containing P8W48, proving that the composite film with seven layers of P8W48 in pH 7 solution showed the optimal electrocatalytic activity for the reduction of 2,4-DNPH. Further, under the optimized conditions, the sensing performance of the P8W48-based composite film was evaluated by CV and i–t curves, giving a linear concentration range of 1 to 700 μM with a low detection limit of 0.012 μM. Moreover, the selectivity, stability, reproducibility and repeatability were examined, confirming that the developed sensor has good potential for determining 2,4-DNPH in the environment.
研究领域:
环境科学
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分析化学
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DOI
高影响因子
NEW JOURNAL OF CHEMISTRY
·
2022
·Vol. 46
·期 43
·20699-20710
·
IF 3.925
Die Wang,Luminita Marin,Xinjian Cheng
Nitro compounds are widely used in modern industries. Among them, 2, 4-dinitrophenylhydrazine (DNH) is extremely harmful. It is of great significance to develop methods for the detection of DNH. In this work, chitosan was used as the substrate material, and fluoroborondipyrrole (BODIPY) was used as the fluorophore. Chitosan was endowed with the fluorescence sensing ability by the introduction of BODIPY units. First, BODIPY derivatives (NO-3 and BO-1) with an alkynyl group (CC) were synthesized. Second, small molecules NO-4 and BO-2 with an aldehyde group (–CHO) were obtained. Finally, the –NH2 groups on chitosan underwent a click reaction (–NH2/CC) and a Schiff base formation reaction occurred (–NH2/–CHO) to form three polymer probes C1, C2 and C3. CC formed in the click reaction can interact with DNH and can be used as recognizing sites for DNH. These chitosan probes have good thermal stability and could selectively recognize DNH, showing notable fluorescence quenching effects, which are visible to the naked eye. DNH is a typical electron-deficient compound, and the polymer fluorescent probe contains electron-rich groups, which makes it easier for the two species to combine and cause fluorescence changes. C1 is flexibly cross-linked, C3 is rigidly cross-linked, and C2 has a non-crosslinked structure, and they show different rheological properties. This work expands the application of chitosan.
研究领域:
材料科学
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环境科学
·
化学
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DOI
高影响因子
ACS Omega
·
2025
·
IF 4.3
Zhenghu Min,Xingdan Wang,Xiaoqiu Yang,Qiwei Zhang,Qi Zheng
Glycosylation profiling is an effective methodology for achieving a comprehensive understanding of glycoproteins and their alterations in a multitude of pathological conditions. However, in comparison to N-glycosylation, O-glycosylation presents significant challenges in terms of both qualitative and quantitative mass spectrometric analyses. A recently developed oxidative release protocol enables the selective formation of O-glycans containing a carboxyl group derived from the amino acid residue. In this study, 3-nitrophenylhydrazine was used to derivatize the common carboxyl group in a mild hydrophilic solution. Derivatization resulted in the generation of a series of report ions for serine, threonine, sialic acid, and O-acetylated sialic acid residues, thereby facilitating the identification of O-glycans and their attached amino acid residues, as well as the determination of the number of O-acetyl groups. A total of 65 O-glycans can be identified from bovine mucin. Furthermore, the analytical strategy revealed that O-acetylated N-acetylneuraminic acid (Neu5Ac)-containing O-glycans from horse serum exhibited distinctive fragmentation patterns in comparison to those from bovine mucin. Additionally, the presence of deaminoneuraminic acid (KDN)-containing O-glycans was successfully confirmed in fish intestinal tissue. These findings suggest that this method provides an economical and potentially valuable tool for large-scale O-glycosylation studies in complex biological samples.
研究领域:
生物化学
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蛋白质组学
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分析化学
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DOI
PubMed
高影响因子
Analytical Methods
·
2018
·Vol. 10
·期 22
·2575-2587
·
IF 2.073
Rui Huang,Wenyan Wu,Shuyu Shen,Jiawen Fan,Yue Chang,Shiguo Chen,Xingqian Ye
The content of flavonoids is important for evaluating the quality of citrus-related products. However, due to the different characteristics of the structures of flavonoids and the lack of a universal method, many methods for quantification have been misused. Here, we used twenty-one citrus flavonoid standards to evaluate four widely used colorimetric methods, and seven species of citrus as natural samples were used to verify the evaluation. The results indicated that NaNO2–Al(NO3)3–NaOH and AlCl3 methods could only detect some of the flavonoids and were inadequate to estimate the total flavonoid content, and the 2,4-dinitrophenylhydrazine (2,4-DNPH) method might be affected by other carbonyl compounds in extracts. The Davis method was modified with naringin as the standard at a measuring wavelength of 420 nm for grapefruit and pomelo, and with hesperidin as the standard at a measuring wavelength of 360 nm for other species. It was proved to be the most reliable method for the quantification of citrus flavonoids and was also recommended for laboratories and factories where needed.
研究领域:
食品科学
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分析化学
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DOI
高影响因子
JOURNAL OF PHOTOCHEMISTRY AND PHOTOBIOLOGY A-CHEMISTRY
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2021
·
IF 4.291
Xinyue Jiao,Luminita Marin,Xinjian Cheng
2,4,6-trinitrophenol (TNP) and 2,4-dinitrophenylhydrazine (DNH) are harmful to the environment and human beings. Trace detection of TNP and DNH is worth of developing facile methods. In this work, cellulose powder and filter paper based fluorescence sensor are synthesized. Firstly, NH 2 CH 2 CH 2 – was introduced into cellulose through etherification reaction, and at the same time, a small molecule BODIPY with –CHO was synthesized. Then BODIPY was incorporated into cellulose by Schiff base reaction to obtain fluorescent macromolecular probes. These fluorescent cellulose sensors can efficiently identify TNP and DNH, with the lowest detection limits of 2.8 × 10 −7 M and 1.6 × 10 −7 M, respectively. Fluorescent filter paper is obtained via the same route. They also exhibit TNP and DNH identification ability. The method developed in filter paper not only expands the application range of cellulose, but also can efficiently identify the pollutants TNP and DNH, which is of great significance in theory and practical applications.
研究领域:
环境科学
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材料科学
·
分析化学
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DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Xiangyuan Zheng,Lan Luo,Jie Zhou,Xiaoling Ruan,Wenyuan Liu,Feng Zheng
s Acyl chlorides are important acylating agents in the synthesis of active pharmaceutical ingredients. Determining the residual acyl chlorides in drug substances is a challenge due to their high reactivity and the matrix interferences from drug substances and their related impurities. This paper describes a general derivatization HPLC method for the determination of aromatic and aliphatic acyl chlorides in lipophilic drug substances. Since most drug substances have weak absorptions in the visible range (above 380 nm), the nitro-substituted anilines and nitro-substituted phenylhydrazines were selected as the derivatization reagents due to their weak basicity and red-shift of UV absorption spectra. The maximum wavelength and absorption intensity of nitro-substituted anilines decreased after derivatization with acyl chlorides, whereas the derivatization products of nitro-substituted phenylhydrazines showed the slight increases of maximum wavelength and absorbance intensity. Hence, 2-nitrophenylhydrazine was selected as the suitable derivatization reagent because the derivatives have the maximum UV wavelength absorbance at 395 nm, which could largely minimize the matrix interferences. The optimization of the concentration of 2-nitrophenylhydrazine is important for the sensitivity and stability of derivatives. Other reaction conditions including reaction temperature, time and the influence of three competitive solvents (water, methanol and ethanol) on the reaction efficiency were also studied. After derivatization with 100 μg mL −1 2-nitrophenylhydrazine at room temperature for 30 min, the method was validated for high specificity and sensitivity with the detection limits in the range of 0.01–0.03 μg mL −1 . The proposed method was applied as a generic method to determine the residual acyl chlorides in lipophilic drug substances.
研究领域:
分析化学
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药学
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DOI
PubMed
高影响因子
TALANTA
·
2019
·
IF 4.916
Huihua Guo,Naizhong Song,Dongze Wang,Jiutong Ma,Qiong Jia
A modulation approach with 4-hydroxybenzhydrazide as the modulating agent was designed for constructing 2,4,6-triphenoxy-1,3,5-benzene-based covalent organic frameworks (COFs). The COFs materials were employed as solid phase microextraction (SPME) coatings for the extraction of phthalate esters (PAEs). Various experimental conditions including extraction temperature, extraction time, salt concentration, and desorption time were investigated and optimized. The introduction of modulating agent into the synthesis of fibers significantly enhanced the extraction efficiency towards PAEs. The linear range was 1–100 μg L ‒1 and the detection limits in the range of 0.032–0.451 μg L ‒1 were achieved with good linearity ranged from 0.9904 to 0.9970. Inter-batch and intra-batch relative standard deviations were in the ranges of 0.83–4.67% and 3.08–9.73%, respectively. Moreover, the developed coating fibers were used for the extraction of PAEs in water samples and satisfactory recoveries were achieved.
研究领域:
分析化学
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材料科学
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产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2023
·Vol. 191
·期 1
·1-11
·
IF 5.7
Guo Zhanghong,Zhou Lin,Chen Xuan,Song Qijun
Carbon-coated copper nanocrystals (CuNCs) with peroxidase-like activity were hydrothermally prepared by using copper acetate, citric acid (CA) and histidine (His) as the precursors. Various shaped CuNCs, including urchin-like, slab-like and spherical appearance were facilely prepared by addition of different amount of NaNO 2 in the precursor solutions. When 3,3′,5,5′-tetramethylbenzidine (TMB) was used as the substrate, the CuNCs with urchin-like appearance have greatest peroxidase-like activity and their Michaelis–Menten constant ( K m ) and the maximum rate constant (ν max ) are respectively 8.8 and 1.2 times higher than that obtained from horseradish peroxidase (HRP). The production of reactive oxygen species (ROS) was confirmed by radical quenching and electron spin resonance (ESR) tests. Subsequent studies have found that the CuNCs catalyzed color reaction of TMB can be selectively quenched by the environmental pollutant 2,4-dinitrophenylhydrazine (2,4-DNPH). Thus a new colorimetric method for the determination of 2,4-DNPH with a linear range of 0.60–20 µM was developed and a limit of detection (LOD) as low as 0.166 µM was achieved. The results obtained not only reveal the tunability of the peroxidase-like activity of Cu-based nanomaterials, but also provide a new method for the sensitive determination of environmental contaminate. Graphical abstract
研究领域:
材料科学
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环境科学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2024
·
IF 2.8
Qian Li,Yongfu Zeng,Lianfeng Ai,Maolin Wei,Xiaomeng Liu,Xiaochan Zhao,Haoran Zhang,Xiujuan Guo
A stable isotope dilution-liquid chromatography tandem mass spectrometry method based on a low-temperature derivatization strategy with 3-nitrophenylhydrazine (3-NPH) was developed for the determination of six volatile fatty acids (VFAs) in serum, urine, and feces. Ice acetonitrile was used to precipitate proteins and extract the target analytes. The extract was derivatized with 3-NPH methanol solution at 4 °C. BEH C8 (1.7 μm, 2.1 × 100 mm) column was used for chromatographic separation, and acetonitrile–water (both containing 0.01 % formic acid) were used as the mobile phase with a gradient elution of 10 min. Electrospray ionization source (ESI) in negative ion multiple reaction monitoring (MRM) mode were used for analyte detection. The regression coefficients R 2 of the calibration curves for the six VFAs were in the range of 0.9963–0.9994, and the LOQs were in the range of 0.02–0.5 μg mL −1 , with the recoveries in the range of 85.3–104.3 %, and the intra- and inter-day precision in the range of 1.8–9.1 %. The method is simple, accurate and reliable, and has been applied in the sensitive determination of VFAs in complex biological samples.
研究领域:
分析化学
·
生物医学
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DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2023
·Vol. 46
·期 20
·2300384
·
IF 3.1
Zheng Jiang,Hong Wang,Miao Yu,Cheng Qu,Wei Yue,Qinan Wu
In this study, a low-cost efficient online derivatization system was developed which allows for the detection of various types of mono- and oligo-saccharides only utilizing high-performance liquid chromatography (HPLC)-ultraviolet detector (UV) system. In the proposed method, phenylhydrazine was used as the derivatization reagent and directly spiked in the mobile phase, allowing for the separation and detection of mono- and oligosaccharides in an accessible instrument system (HPLC-UV). And the online derivatization design of the proposed method has significantly reduced the potential harm of derivatization reagents to the analysts. Furthermore, critical chromatographic parameters were optimized via the Box-Behnken design strategy, culminating in the ideal response for saccharides. Finally, the methodology validation of the proposed method was conducted. The proposed method showed satisfactory linear ranges with acceptable correlation coefficients (R 2 > 0.99), outstanding accuracy (Recovery: 95.3%–105.6%), high intra-day precision (relative standard deviation [RSD]: 1.4%–7.1%) and inter-day precision (RSD: 2.0%–7.4%). The robustness and ruggedness of the proposed method were proved as the recovery values in the range of 95.0%–104.6% and 95.1%–104.8% for robustness and ruggedness, respectively. These satisfactory validation results confirm the applicability and reliability of the proposed method for the analysis of saccharides in various complex real-world samples.
研究领域:
分析化学
·
食品科学
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产品关联
DOI
PubMed
高影响因子
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