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TALANTA · 2015 · IF 3.545

Direct and simultaneous quantification of ATP, ADP and AMP by 1H and 31P Nuclear Magnetic Resonance spectroscopy

Yakun Lian,Hua Jiang,Jinzhou Feng,Xiaoyan Wang,Xiandeng Hou,Pengchi Deng

ATP , ADP and AMP are energy substances with vital biological significance. Based on the structural differences, a simple, rapid and comprehensive method has been established by 1 H and 31 P Nuclear Magnetic Resonance ( 1 H-NMR and 31 P-NMR) spectroscopies. Sodium 3-(trimethylsilyl) propionate-2,2,3,3-d 4 (TMSP) and anhydrous disodium hydrogen phosphate (Na 2 HPO 4 ) were selected as internal standards for 1 H-NMR and 31 P-NMR, respectively. Those three compounds and corresponding internal standards can be easily distinguished both by 1 H-NMR and 31 P-NMR. In addition, they all have perfect linearity in a certain range: 0.1–100   mM for 1 H-NMR and 1–75   mM for 31 P-NMR. To validate the precision of this method, mixed samples of different concentrations were measured. Recovery experiments were conducted in serum (91–113% by 1 H-NMR and 89–113% by 31 P-NMR).

研究领域: 生物化学 · 医学检测
✓ 已验证 DOI PubMed 高影响因子
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Separations · 2022 ·Vol. 9 ·期 6 ·140 · IF 3.344

Quantitative Analysis of Anthocyanins in Grapes by UPLC-Q-TOF MS Combined with QAMS

Xue Li,Wei Wang,Suling Sun,Junhong Wang,Jiahong Zhu,Feng Liang,Yu Zhang,Guixian Hu

A method for quantifying the anthocyanins in grapes was firstly developed by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOFMS) combined with quantitative analysis of multi-components by single marker (QAMS). A total of 10 main anthocyanins were analyzed by using peonidin 3-O-glucoside as the reference standard. The accuracy of this method was evaluated by an established and validated external standard quantification method with 10 reference compounds. The standard method difference (SMDs) of the quantification results between QAMS and the external standard methodwasless than 15%. Furthermore, the QAMS method was used to analyzefour batches of grapes and the data was compared with those obtained using the external standard method. No significant difference wasobtained in the results obtained by both methods. These results indicated that the QAMS method could accurately determine the anthocyanins in grapes. This method can provide a basis to address the absence of reference standards for analyzing anthocyanins in other foods.

研究领域: 食品科学 · 分析化学 · 植物学
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MOLECULES · 2023 ·Vol. 28 ·期 5 ·2022 · IF 4.6

UPLC-MS Analysis, Quantification of Compounds, and Comparison of Bioactivity of Methanol Extract and Its Fractions from Qiai (Artemisia argyi Lévl. et Van.)

Ting Zhang,Dingrong Wan,Yuanyuan Li,Sisi Wang,Xiuteng Zhou,Fatemeh Sefidkon,Xinzhou Yang

TheArtemisia argyiLévl. et Van. growing in the surrounding areas of Qichun County in China are called Qiai (QA). Qiai is a crop that can be used both as food and in traditional folk medicine. However, detailed qualitative and quantitative analyses of its compounds remain scarce. The process of identifying chemical structures in complex natural products can be streamlined by combining UPLC-Q-TOF/MS data with the UNIFI information management platform and its embedded Traditional Medicine Library. For the first time, 68 compounds in QA were reported by the method in this study. The method of simultaneous quantification of 14 active components in QA using UPLC-TQ-MS/MS was reported for the first time. Following a screening of the activity of QA 70% methanol total extract and its three fractions (petroleum ether, ethyl acetate, and water), it was discovered that the ethyl acetate fraction enriched with flavonoids such as eupatilin and jaceosidin had the strongest anti-inflammatory activity, while the water fraction enriched with chlorogenic acid derivatives such as 3,5-di-O-caffeoylquinic acid had the strongest antioxidant and antibacterial activity. The results provided the theoretical basis for the use of QA in the food and pharmaceutical industries.Keywords:Artemisia argyiLévl. et Van.;UPLC-MS;quantification;anti-inflammatory;antioxidant

CAS / MDL: 67-68-5
研究领域: 药理学 · 分析化学 · 传统医学
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ANALYTICA CHIMICA ACTA · 2019 · IF 5.256

NMR analysis of the Fischer-Tropsch wastewater: Combination of 1D selective gradient TOCSY, 2D DOSY and qNMR

Hui Ma,Christian Marcus Pedersen,Qi Zhao,Zexiang Lyu,Hui Chang,Yan Qiao,Xianglin Hou,Yingxiong Wang

The Fischer–Tropsch (FT) process is a practical approach to convert synthesis gas (CO and H 2 ) into hydrocarbons and oxygenates, and these product mixtures are usually well-characterized. However, the analysis of Fischer–Tropsch waste water (FTW) is still somewhat underdeveloped and the exact composition of FTW remains unclear. Herein, various qualitative NMR techniques, especially diffusion-ordered spectroscopy (DOSY) and one dimension (1D) selective gradient total correlation spectroscopy (SelTOCSY) were strategically applied in the analysis of FTW. The NMR results show that the DOSY technique can pseudo-separate most of components in complex mixtures over the diffusion dimension. The SelTOCSY technique is used as a supporting method in the cases where the DOSY technique cannot clearly distinguish overlapped signals. Moreover, the quantitative 1 H NMR (qNMR) was further used to quantify the components of the sample. These routine and advanced qualitative and quantitative NMR technique utilized here provide a fast, effective and feasible method for the identification of complex mixtures in FTW, which might be a powerful and fast alternative to gas chromatography or high performance liquid chromatography for FTW research.

研究领域: 化学 · 环境科学
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JOURNAL OF RARE EARTHS · 2023 · IF 4.9

Quantitative discrimination of surface adsorbed NOx species on CeO2 via spectrophotometry for SCR denitration investigation

Songil Sin,Jiawei Ji,Lijun Cheng,Zhiwen Gu,Chong Tan,Kwangchol Ri,Changjin Tang

CeO 2 -based catalysts are widely investigated for selective catalytic reduction (SCR) of NO with NH 3 . Interaction of NO/O 2 with CeO 2 generally produces two surface species, i.e., nitrates and nitrites. However, the explicit quantification of these two species is still unresolved. Herein, we reported that spectrophotometry characterization was effective in determining surface adsorbed NO x species on CeO 2 by measuring the corresponding ions (NO 2 – and NO 3 – ) dissolved in aqueous solution. Experimental results show that both nitrate (–NO 3 ) and nitrite (–NO 2 ) species can be quantitatively evaluated and the accuracy is verified by calibrating with NO x -TPD result. Exclusive transfer of adsorbed NO x from catalyst surface to aqueous solution is confirmed and the dissolution process can be accelerated by ultrasonic treatment. Moreover, useful information related to evolution of surface NO x species under various conditions (O 2 treatment, different adsorption temperature and duration) and over different catalysts (Fe 2 O 3 , MnO 2 and MnO x –CeO 2 ) are provided. The result of present study demonstrates the potential of spectrophotometry for quantitative discrimination of surface NO x species on CeO 2 and other oxide-based materials, which is conducive to mechanism analysis of SCR reaction.

研究领域: 催化化学 · 环境科学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2018 · IF 2.831

Rapid quantification of polysaccharide and the main onosaccharides in Dendrobium huoshanense by near-infrared attenuated total reflectance spectroscopy

Jing-Wen Hao,Nai-Dong Chen,Cun-Wu Chen,Fu-Cheng Zhu,De-Liang Qiao,Yong-Jun Zang,Jun Dai,Xiang-Wen Song,Han Chen

A rapid, green, low cost and nondestructive attenuated total reflection near infrared (ATR NIR) method was developed to quantify the total polysaccharide and the main monosaccharides mannose and glucose in Dendrobium huoshanense. Total 100 D. huoshanense samples from different places were analyzed using ATR NIR method. Potential outlying samples were initially removed from the collected NIR data using the PCA-Mahalanobis distance method. Spectral data preprocessing was studied in the construction of a partial least squares (PLS) model and six different signal pretreatment methods, including multiplicative scattering correction (MSC), standard normal transformation (SNV), first and second derivatives, the combination of MSC with the first derivative, and the combination of SNV with the first derivative, were compared. The results showed that the best signal pretreatment method was the spectral data pretreated by SNV combined with the first derivative due to it showed the lowest root-mean-square error of cross-validation (RMSECV), highest R 2 for both the polysaccharide and its main monosaccharides . In order to improve the performance of the model, the pretreated full spectrum was calculated by different wavelength selection method. The results showed that the optional wavelength selection model was the one simultaneously selecting the NIR wavelength ranges 7500–5750 cm −1 , 5250–4700 cm −1 , 4450–4300 cm −1 and 4200–4100 cm −1 because of the lowest RMSECV and the highest R 2 among the ten wavelength selection models. The external validation and the complete external validation confirmed the robustness and reliability of the developed NIR model. The contents of the total polysaccharide and the main monosaccharides are the essential quality assessment criterion for plant medicines while their traditional quantification methods involved sample destruction, tedious sample processing and non-environmentally friendly pretreatment, therefore, our study might provide an efficient technique tool for the rapid, green and nondestructive quantification of the total polysaccharide and the main monosaccharides for D. huoshanense and other rich-in-polysaccharide plant medicines.

研究领域: 植物学 · 分析化学 · 药学
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RSC Advances · 2021 ·Vol. 11 ·期 37 ·23002-23009 · IF 3.361

Development and comparison of UPLC-ESI-MS and RP-HPLC-VWD methods for determining microcystin-LR

Peng Jin,Kai Yang,Ruining Bai,Mei Chen,Shilin Yang,Kebo Fu,Jieli He

Microcystin-LR (MC-LR) generated by cyanobacteria is a kind of potent hepatotoxin, which poses a considerable threat to human health. In the research field of MC-LR removal, the quantitative analysis in a wide concentration range of samples is inevitable. In this paper, we presented the pseudo united use of an Ultra Performance Liquid Chromatography Mass Spectrometry (UPLC-MS) and High Performance Liquid Chromatography system with a Variable Wavelength Ultraviolet Detector (HPLC-VWD) approach to detect MC-LR. The UPLC-MS system was applied to determine MC-LR in trace concentration because of its high sensitivity. However, it is generally believed that the determination of high concentration samples by UPLC-MS will cause problems such as inaccurate quantification and contamination of ion sources. In consequence, the HPLC-VWD was employed to determine the high concentration of MC-LR. The sensitivity, precision and accuracy of the two methods were compared in detail. The linear ranges of UPLC-MS and HPLC-VWD methods were from 0.08 to 10 μg L−1 and 1 to 5000 μg L−1, respectively. The detection and quantification limits of UPLC-MS were 0.03–0.05 μg L−1 and 0.08 μg L−1, and the corresponding two values of HPLC-VWD were 0.6 and 1.0 μg L−1. The recoveries of UPLC-MS and HPLC-VWD were 88.5–106.7% and 98.7–101.6%, with the relative standard deviations of 3.72–5.45% and 0.38–1.69%, respectively. The potential adsorption properties of MC-LR on filter membranes with diverse materials and pore sizes were evaluated and the negative results were obtained. The detection of MC-LR by UPLC-MS was free from matrix effects. The presented UPLC-MS and HPLC-VWD methods were used to analyze the water samples from Erhai Lake, which is located in Dali, Yunnan, China. The results of UPLC-MS analysis indicated that the MC-LR was only identified in water samples of Shuanglang Bay and Xier River, with concentrations of 0.120 and 0.303 μg L−1, whereas MC-LR was not detected by HPLC-VWD.

研究领域: 环境科学 · 毒理学 · 分析化学
✓ 已验证 DOI PubMed 高影响因子
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2022 · IF 3.571

Matrix-assisted laser desorption/ionization mass spectrometric imaging the spatial distribution of biodegradable vascular stents using a self-made semi-quantitative target plate

Houwei Lin,Yinlian Yuan,Tian Hang,Peng Wang,Shijiao Lu,Hang Wang

In recent years, the development and optimization of biodegradable coronary stents have become the research focus of many medical device manufacturers and scientific research institutions since they can be completely degraded and absorbed, and they restore vascular function. However, there is a lack of in situ quantification of these stents spatially in tissue in vivo . In this study, matrix-assisted laser desorption/ionization (MALDI) Fourier transform ion cyclotron resonance (FT ICR) and time-of-flight (TOF) mass spectrometric imaging (MSI) were used to analyze the time-dependent distributions of a biodegradable vascular scaffold, which consisted of copolymers of lactic acid and glycolic acid (PLGA) and its degradation products in cross-sections and longitudinal sections of blood vessels. The MALDI-MSI methods for analyzing the distribution of PLGA and its derivatives in vivo were established by optimizing the conditions of sample pretreatment and mass spectrometry (MS). In order to semi-quantify the contents of PLGA degradation products in blood vessels, self-made stainless-steel and indium tin oxide (ITO) target plates were developed to compare and establish the standard curves for semi-quantitative analysis. The target plate can be placed on the target carrier of MS simultaneously with the conductive slide, which can simultaneously carry out vapor deposition or spray on the substrate, to ensure the parallelism of the pretreatment experiments between the standards and the actual vascular samples. The proposed method provided a powerful tool for evaluating the distributions and degradation process of biological stent materials in the coronary artery, as well as provided technical support for the research and development of degradable biological stents and product optimization.

研究领域: 医学影像学 · 材料科学 · 生物医学工程
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Analytical Methods · 2013 ·Vol. 5 ·期 22 ·6395-6400 · IF 1.855

Determination of nucleosides and nucleobases in Isatidis Radix by HILIC-UPLC-MS/MS

Yilin Pan,Ping Xue,Xiang Li,Jianwei Chen,Jin Li

To establish an ultra-high performance liquid chromatography coupled with triple quadrupole mass (HILIC-UPLC-MS/MS) for determination of sixteen nucleosides and nucleobases in Isatidis Radix. Chromatographic separation was carried out on a Acquity UPLC BEH Amide column with gradient elution of acetonitrile (containing 0.1% acetic acid) and water (containing 0.8% acetic acid and 10 mmol L−1 ammonium acetate) at a flow rate of 0.3 mL min−1, the column temperature was set at 35 °C; Waters Xevo™ TQ worked in multiple reaction monitoring mode. Each component were separating in 11 min. All calibration curves were linear (r2 > 0.997) over the tested ranges. The limits of detection of these compounds were 0.02–42.54 ng mL−1. The limits of quantitation of these compounds were 0.05–98.18 ng mL−1. The average recoveries were in the range of 93.81–105.77% with RSD value less than 7.5%. The result showed that almost all of these Isatidis Radix were rich in nucleosides and nucleobases, but their contents were obviously various. The method was simple and fast with high precision, sensitivity and repeatability, which can be used for determination of this type class of nucleosides and nucleobases in other medicinal herbs.

研究领域: 药学 · 分析化学
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JOURNAL OF CHROMATOGRAPHIC SCIENCE · 2021 ·Vol. 59 ·期 10 ·941-948 · IF 1.618

New Determination Method of Two Bioactive Saponins in Lysimachia capillipes Hemsl. by Quantitative Analysis of Multi-Components by Single-Marker

Zhang Xiaoyong,Chen Xuezhao,Jin Juan,Gong Minghua,He Qiang,Li Shouxin,Tian Jinkui

Capilliposide B (CPS-B) and Capilliposide C (CPS-C), as the key components in Lysimachia capillipes Hemsl., increasingly aroused the interest and research concern of many researchers due to the good bioactivities. Nowadays, the reference standards of CPS-B and CPS-C yield were very limited. Due to the deficit of reference standards, the determination could be difficult to carry out, and the quality control and evaluation would be restrained afterwards. To solve this urgent problem, a quantitative analysis of multi-components by single-marker (QAMS) method was proposed and established based on high-performance liquid-chromatography tandem evaporative light-scattering detector. In this QAMS method, the content of the two bioactive components could be calculated by buddlejasaponin IV, which is applied as an external standard and readily obtained. And the methodological experiments were evaluated and indicated accuracy, stability and feasibility of this QAMS method. Therefore, in this study, this built method would properly meet the requirement of determination of CPS-B, CPS-C and quality control of the L. capillipes Hemsl. plant.

CAS / MDL: 64-19-7
研究领域: 植物化学 · 药物分析
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EUROPEAN FOOD RESEARCH AND TECHNOLOGY · 2021 ·Vol. 247 ·期 11 ·2687-2698 · IF 2.998

Quantitative and fingerprint analysis of proanthocyanidins and phenylpropanoids in Cinnamomum verum bark, Cinnamomum cassia bark, and Cassia twig by UPLC combined with chemometrics

Liu Chen,Long Huali,Wu Xingdong,Hou Jinjun,Gao Lei,Yao Shuai,Lei Min,Zhang Zijia,Guo De-an,Wu Wanying

Cinnamomum verum and Cinnamomum cassia are widely used as spice and herbal medicine around the world. However, it is challenging to differentiate and make a quality evaluation for both Cinnamomum types due to their similarities in morphological features and general chemical composition using traditional analytical methods. In this study, a simple and efficient method was developed for the comprehensive evaluation of the two Cinnamomum, together with Cassia twig, by combining UPLC fingerprint analysis combined with quantitative analysis using two internal standards for the determination of multiple components (TSDMC). The content of 9 components (procyanidin B2, cinnamtannin B1, coumarin, 2-hydroxycinnamaldehyde, cinnamyl alcohol, cinnamic acid, cinnamaldehyde, 2'-methoxycinnamaldehyde, and eugenol) in samples was determined using reliable relative conversion factor factors that were obtained using procyanidin B2 and cinnamic acid as two internal reference standards. The quantitative results combined with chemometrics analysis were employed to identify these samples. This simple and reproducible method revealed great differences among the three Cinnamomum in their chemical composition and provides a promising method for accurate differentiation and quality evaluation for the three Cinnamomum.

研究领域: 药学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2022 · IF 3.318

A rapid UHPLC-QDa method for quantification of human salivary amino acid profiles

Chun Qu,Chaohui Jian,Kun Ge,Dan Zheng,Yuqian Bao,Wei Jia,Aihua Zhao

Abnormal salivary amino acid (AA) levels may indicate dysfunction of the body. Being noninvasive, sampling easily and cost-effective of saliva, a rapid, precise and simple analysis method has become very important for quantitative salivary AA profiles. After one-step to precipitate protein, the resultant extraction was derived with 6-aminoquinolyl- N -hydroxysuccinimidyl carbamate (AQC) within 10 min. Quantitation of AA profile was achieved within 6 min in a single run by ultra-high performance liquid chromatography coupled with a single quadrupole mass spectrometry (UHPLC-QDA detector). The method was validated with acceptable accuracy ranging from 80.33 % to 122.31 %, appropriate linearity with the coefficient (R 2 ) more than 0.991, good intra- and inter-day precision, repeatability and stability (RSD < 15 %). The recoveries at three different spiked concentrations ranged over 79.18 %–125.36 % while the matrix effect was from −19.86 % to 11.95 %. This simple, rapid and robust method was successfully applied to quantify human salivary 30 amino acids, in which the levels of taurine, γ-aminobutyric acid, methionine and tryptophan in healthy people were close to the LOQs. Besides, the levels of histidine and cystine were not able to be measured due to their relatively high LOQs, which were considered as the limitations of this developed method.

CAS / MDL: 148757-94-2
研究领域: 分析化学 · 生物医学
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