PHYTOCHEMICAL ANALYSIS
·
2022
·Vol. 33
·期 4
·577-589
·
IF 3.024
Xiao-Lei Miao,Hui-Min Ma,Qin-Hao Ke,Shi-Yue Wang,Hong-Fu Zhou,Min Zheng
Aim To establish a fast, sensitive and accurate high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for determining the monosaccharide content of Qingzhuan Dark Tea polysaccharides in different years (2 years, 5 years and 11 years). Methods The optimised chromatographic conditions were achieved on a C18 column (5.0 μm, 250 mm × 4.6 mm inner diameter). The mobile phase flow rate was 0.9 mL/min and the column temperature was set to 27°C. The aqueous phase A (5 mM aqueous ammonium acetate) and organic phase B (acetonitrile) were used to elute the target analyses isocratically (0–60 min: 18% B). The mass spectrometer detector was equipped with an electron spray ionisation (ESI)source, and multiple reaction monitoring (MRM) mode was used for the determination of 1-phenyl-3-methyl-5-pyrazolone (PMP) derived monosaccharides. Results We carried out a comprehensive methodological validation of PMP derived monosaccharides, including linearity, precision, stability and repeatability. Nine monosaccharides (rhamnose, mannose, ribose, glucose, galacturonic acid, xylose, galactose, fucose and arabinose) of Qingzhuan Dark Tea polysaccharides were identified, in which ribose and fucose were reported for the first time. The results showed the contents of these nine monosaccharides differed significantly among different years. Conclusions The validated method is reliable, accurate, repeatable and can be applied to quality assessment of these monosaccharides.
研究领域:
食品科学
·
分析化学
·
植物化学
✓ 已验证
DOI
高影响因子
Separations
·
2023
·Vol. 10
·期 9
·515
·
IF 2.6
Xiaodong Wang,Wenhao Wang,Qinggui Lei,Zhengming Qian,Wenbin Deng
This study aims to develop a fast and eco-friendly liquid chromatography–mass spectrometry (LC-MS) method for the determination of aesculin and aesculetin in Cortex Fraxini. Ultrapure water was used as the solvent during the microwave-assisted extraction process to prepare the Cortex Fraxini sample. This extraction method reduces the cost of the harmful solvent (only ultrapure water was used) and microwave extraction time (1 min). The LC separation was conducted using an Agilent InfinityLab Poroshell 120 EC-C18column (2.1 mm × 30 mm, 2.7 µm) with a mobile phase consisting of 0.1% formic acid and acetonitrile (90:10,v/v) at a flow rate of 0.6 mL/min. Isocratic elution was employed, and the analytes were detected by MS. Through careful optimization and selection of LC-MS conditions, the analysis time was reduced to 1 min, demonstrating the method’s efficiency. The developed method was validated and exhibited excellent specificity, linearity, limit, precision, accuracy, and stability in quantifying aesculin and aesculetin in the Cortex Fraxini samples. The analysis result revealed the presence of aesculin (ranging from 3.55 to 18.8 mg/g) and aesculetin (ranging from 1.01 to 16.2 mg/g) in all ten batches of Cortex Fraxini samples. Compared to the reported LC methods, this approach substantially reduces the total analysis time and requires a minuscule volume of organic solvents. An “Analytical Eco-Scale” assessment was used to evaluate the different assay methods of Cortex Fraxini. The current LC-MS method scored an impressive 90; it was better than the other four reports’ LC methods. Thus, the developed LC-MS method is rapid and green, which is helpful for the quality evaluation of Cortex Fraxini.Keywords:LC-MS;Cortex Fraxini;aesculin;aesculetin;green;fast
研究领域:
药学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
Food Quality and Safety
·
2022
·
IF 3.949
Kang Yuting,Li Chenghua,Li Huiru,Li Jing,Jiang Kezhi
Polycarboxylic acids (PACs) are important metabolic products in almost all living bodies, yet current analytical methods for detection of PACs in tea beverages are still unsatisfactory due to the complex matrix and physicochemical properties of PACs. In this work, a rapid method was developed for the simultaneous determination of 7 PACs, including tartaric acid, α-ketoglutaric acid, malic acid, malonic acid, cis-aconitic acid, succinic acid, and fumaric acid, in beverages, based on selective removal of the matrix in combination with liquid chromatography–mass spectrometry (LC-MS) analysis. By stirring with activated carbon and the Na2CO3 solution, the matrix in beverages was selectively removed, and PACs were almost retained in the supernatant of diluted Na2CO3 solution. Under optimized parameters, the limit of quantitation for the PACs was in the range of 1–50 ng/mL, and the content of the PACs in 8 beverages was determined with the recovery range of 72.2%–122.5%. The contents of malic acid, malonic acid, and succinic acid in tea beverages were found to be greater than those in non-tea beverages. Moreover, the concentration of these PACs in beverages was found to be multiplied many times in their deterioration period, especially for fumaric acid and α-ketoglutaric acid. These results indicated that PACs can be selected as a criterion to differentiate qualified tea beverages from spoiled beverages.
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
CHINESE CHEMICAL LETTERS
·
2022
·
IF 8.455
Hao Gu,Guoxin Dai,Siyu Liu,Yanbing Zhai,Qian Xu,Hongqiang Wu,Wei Xu
Liquid chromatography tandem mass spectrometry (LC-MS/MS) plays an important role in clinical diagnostics. Although LC-MS/MS is superior in terms of accurately quantifying molecules in complex matrices, instrument footprint, operation and maintenance complexity also hinder its expansion as the analytical technique of choice. In this study, a compact LC-MS instrument was developed, in which an assembled liquid chromatograph was coupled with a miniature ion trap mass spectrometer. The overall instrument has a footprint of 69 cm × 31 cm × 31 cm, and it requires no gas supply as well as minimum maintenance. Furthermore, the use of LC-MS is in accord with conventional clinical diagnostic protocols, and the choice of ion trap offers tandem MS performance. The results showed that the use of LC could improve both mixture analysis capability and detection sensitivity of the miniature mass spectrometer. After optimization, feasibility of this instrument in clinical practice was demonstrated by the quantitation of four widely used immunosuppressants in blood samples. Relatively good linearities were obtained, which spanned the reference ranges of effective therapeutic concentrations of each immunosuppressant. Intra-day and inter-day accuracy and precision of analytical method were also assessed. This work showed that a compact LC-MS instrument could be used in clinical diagnosis, either to replace conventional lab-scale instruments or to be used in POCT applications.
研究领域:
分析化学
·
医学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2022
·Vol. 45
·期 22
·4099-4106
·
IF 3.614
Suling Zhang,Ziluo Hua,Weixuan Yao,Ting Lü,Dong Zhang,Hongting Zhao
In this study, magnetic pomelo peel-derived biochar composite was fabricated and applied as a low-cost adsorbent for the simultaneous extraction of morphine-like opioids named morphine, codeine, and 6-monoacetylmorphine from wastewaters, prior to their determination via liquid chromatography-mass spectrometry. A total of four biochar products were synthesized under different pyrolytic temperatures of 400, 500, 600, and 700°C, respectively, and the 400°C biochar was found to have the greatest extraction ability, with enrichment factors of 34, 58, and 61 for the three drugs. The primary adsorption mechanism includes π-π interaction and H-bonding. Parameters affecting the extraction of opioids were optimized. Under optimum conditions (such as pH = 7; adsorbent amount = 15 mg; sample volume = 20 ml; eluent solvent, 200 µl of methanol), the method was proved to be linear in the range of 0.05–10.0 µg/L, with coefficients of determination greater than 0.99, and the limits of detection were 0.006–0.010 µg/L. In-batch and inter-batch precisions were 1.8%–6.5% and 4.8%–10.6%, respectively. The method was successfully applied to the determination of the target opioids in the samples of influent and effluent wastewater. The developed method by using magnetic pomelo peel-derived biochar could potentially be applied for the effective estimation of illicit drug consumption.
研究领域:
环境科学
·
分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
·
2014
·
IF 3.107
Yan-Wen Li,Xiao-Jing Zhan,Lei Xiang,Zhe-Shen Deng,Bin-Hui Huang,Hong-Fei Wen,Teng-Fei Sun,Quan-Ying Cai,Hui Li,Ce-Hui Mo
A selective and sensitive method for the simultaneous detection of three common and hazardous microcystins (microcystins-LR, -RR, and -YR) in various vegetables was established using solid-phase extraction followed by high performance liquid chromatography coupled with mass spectrometry. The methanol–water proportion ratio of the extraction solvent and its acidity, as well as the efficiencies of solid-phase extraction, were evaluated to optimize a pretreatment procedure for extracting the microcystins from 10 vegetable matrices. The limits of detection and quantitation were below 7.5 μg/kg (dw) and 25 μg/kg (dw), respectively, in different vegetable matrices. The recoveries of the microcystins in the 10 vegetable matrices ranged from 61.3 to 117.3%, with RSDs of 0.2–18.3%. The established method was used to analyze 28 field vegetable samples collected from the sides of Lake Dianchi, and microcystin-RR was found in almost all samples at concentrations of 36.4–2352.2 μg/kg (dw).
研究领域:
环境科学
·
食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS
·
2018
·
IF 3.468
Jin Zong You,Cheng Jie Wu,Xue Jie Wang
Irbesartan (IBS) is an inhibitor of angiotensin II receptor. In order to study the thermal stability and the thermal decomposition mechanism of IBS, the thermal decomposition processes of IBS in nitrogen and in air atmospheres were studied by means of thermogravimetry (TG) and differential scanning calorimetry (DSC), the evolved gaseous products from thermal decomposition were identified with thermogravimetry coupled with Fourier transform infrared spectroscopy (TG-FTIR), and the residues of thermal decomposition at various temperatures were analyzed with infrared spectra, high-performance liquid chromatography (HPLC) and liquid chromatography-mass spectrometry (LC–MS). The molecular bond orders were calculated by GAMESS program of quantum chemistry, and the thermal decomposition mechanism of IBS was discussed. The results indicated that the thermal decomposition of IBS is a three-stage process and the initial temperatures of the decomposition are 204.7 and 201.0 °C in nitrogen and in air, respectively. The initial step of the decomposition is the partial decomposition of imidazolone and tetrazol sections. The thermal stability of IBS is quite good in the routine temperature.
研究领域:
药学
·
分析化学
·
量子化学
✓ 已验证
DOI
高影响因子
INTERNATIONAL JOURNAL OF FOOD PROPERTIES
·
2016
·
IF 1.586
Kechan Lei,Wanxing Wei,Sheng Liu,Min Zhou,Xiaoxia Lin,Xun Cao
Antioxidant activities of the extract containing anthocyanins from fruit of Sageretia theezans Brongn were investigated in this work. The fruit of Sageretia theezans Brongn was treated with 0.001 mol·L–1 HCl in a solid (g): liquid (mL) ratio 1:10 to give extract. Total anthocyanins content was 253.10 ± 2.31 mg in 100 g fruit. The anthocyanins in extract were determined as cyanidin-3-sophorose-5-glucoside (Cy-3-Sp-5-Glu), petunidin-3-(6′-malonyl)-glucoside (Pt-3-(6’-Mal)-Glu), malvinidin-3-glucosid (Mv-3-Glu), and peonidin-3-(6′-malonyl)-glucoside (Pn-3-(6’-Mal)Glu) in 0.38, 22.57, 44.32, and 30.86%, respectively, by high performance liquid chromatography-mass spectrometry method. Antioxidant activities of the anthocyanins in extract were evaluated by methods of ferric reducing antioxidant power, hydroxyl radical scavenging assay, and superoxide radical scavenging assay. The anthocyanins in extract exhibited obvious antioxidative activities. These results suggested that the fruit of Sageretia theezans Brongn could be considered as a good source of natural antioxidants.
研究领域:
植物化学
·
食品科学
·
药理学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2022
·Vol. 45
·期 13
·2128-2139
·
IF 3.614
Li Zhang,Qing Hu,Jie Wang,Huamin Zhang,Jiangbin Han
Budesonide is an active pharmaceutical ingredient used in various dosage forms of finished products for the treatment of asthma. During the process of drug development, unbiased analysis of related substances is of utmost significance for both pharmaceutical research and quality control purposes. In this work, the official method documented in the United States Pharmacopoeia was selected to determine the related substances of budesonide considering the pros and cons of critical chromatographic parameters, compared to the European Pharmacopoeia. In doing so, several unpredictable interference peaks, namely “ghost peaks”, were observed occasionally during analysis. A strategy that integrated information derived from experimental operation inspection, liquid chromatography/mass spectrometry fingerprint analysis, and mechanism-based stress studies was then proposed for comprehensively and quickly exploring those non-degradable and degradable peaks. Some ghost peaks were found to originate from nylon syringe filter, illumination, and alkali borosilicate glass high-performance liquid chromatography vials. Besides, degradation pathways under alkaline conditions were also unraveled through liquid chromatography-mass spectrometry qualitative analysis. Overall, an optimization of the analytical methodology based on the United States Pharmacopoeia for its application in impurity analysis of budesonide and corresponding formulations was carried out with the design of experiments, by which “ghost peaks” could be suppressed or prevented. The results obtained herein are not only crucial to studies on budesonide's stability or degradation kinetics but also contribute to clarifying the impurity research of other drugs.
研究领域:
药物分析
·
制药工程
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2022
·Vol. 46
·期 2
·2200311
·
IF 3.614
Zhien Tan,Shimin Chen,Mengli Zhang,Xiaosheng Qu,Taiping Li,Aihua Zhang,Yanmei He,Min Ou,Lihuo Long,Lu Chen,Fangfang Wu
Abrus mollis Hance is a traditional Chinese medicine that is widely used to treat acute and chronic hepatitis, steatosis, and fibrosis. Its therapeutic qualities of it have long been acknowledged, although the active ingredients responsible for its efficacy and the mechanisms of its action are unknown. In this study, the chemical constituents absorbed into the blood from Abrus mollis Hance were assessed by using liquid chromatography-quadrupole-time-of-flight mass spectrometry and the data was analyzed with the UNIFI screening platform. The results obtained were compared to existing chromatographic-mass spectrometry information, including retention times and molecular weights as well as known reference compounds. 41 chemical constituents were found in Abrus mollis Hance, and these included 16 flavonoids, 13 triterpenoids, five organic acids, and two alkaloids. Experimentally it was found that Abrus mollis Hance had a therapeutic benefit when treating α-naphthalene isothiocyanate-induced acute liver injury in rats. In addition, 11 blood prototypical constituents, including six flavonoids, three triterpenoids, and two alkaloids, were found in serum samples following intragastric administration of Abrus mollis Hance extracts to rats. This novel study can be used for the quality control and pharmacodynamic assessment of Abrus mollis Hance in order to assess its efficacy in the therapeutic treatment of patients.
研究领域:
中药学
·
分析化学
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2022
·
IF 4.52
Meng Dong,Ran Xin,Zhi-Yuan Li,Yu-Lian Li,Xu-Hui Huang,Xiu-Ping Dong,Bei-Wei Zhu,Lei Qin
The organic acids in fruits have critical impacts on palatability and flavor . In this paper, we established a method to quantify 21 essential organic acids in animal and plant matrices using HPLC mass spectrometry with high sensitivity and broad applicability. The organic acids in 12 animal and plant matrices were quantified. Additionally, the profile and concentration of organic acids could achieve the classification of samples. The fruit quality traits and important organic acids content during the storage of cherry tomatoes were monitored via our method. Nine organic acids changed significantly in 16 days of storage, especially citric acid , as the most predominant organic acid, decreased from 4260 to 2290 μg/g, leading to a decline in sourness of 46.2 %. In contrast, after 16 days of storage, galacturonic, gluconic, malonic and quinic acids increased by 155 %, 88 %, 162 %, and 112 %, respectively, which had a potential effect on softening and deteriorating of cherry tomatoes.
研究领域:
食品科学
·
植物生理学
✓ 已验证
产品关联
DOI
高影响因子
CHROMATOGRAPHIA
·
2017
·Vol. 80
·期 12
·1733-1739
·
IF 1.402
Zhang Chaozheng,Zheng Yu,Ma Shenxi,Wu Zhiguo
Abstract Bile acids are essential materials in the fatty acid cycle. Thus, understanding the metabolism of bile acids is significant. In this study, LC–MS was employed to analyze the composition and content of bile acids in rat cecal contents. Six individual bile acids were determined simultaneously. The mobile phase consisted of acetonitrile and 10 mmol L −1 of ammonium acetate solution. The flow rate was 0.2 mL min −1 , and the total analysis time was 34 min. Under the developed conditions, all calibration curves for the six individual bile acids were achieved, and all correlation coefficients exceeded 0.99. Meanwhile, satisfactory results were obtained in the range of 50–500 µg g −1 for the six individual bile acids in the rat cecal contents. The LOD and LOQ of the bile acids were as low as 2.5 and 10 µg g −1 in the rat cecal contents, respectively, and the relative standard deviations of the peak area were within 1.25–2.01%. The dried residues after extraction were selected as the blank matrix. The overall recovery efficiencies of the bile acids in biological samples were increased to 97.2–103.2%. Therefore, the developed method can be used to quantify individual bile acids at extremely low levels in rat cecal contents. Graphical Abstract
研究领域:
生物化学
·
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）