MICROCHEMICAL JOURNAL
·
2022
·
IF 5.304
Chu Chu,Linmin Lian,Wei Gao,Yaping Zang,Yanfang Zou,Yangbin Lv,Chenyue Li,Shengqiang Tong,Jizhong Yan,Suhong Chen
An efficient off-line and on-line synergistic preconcentration strategy which involves combining micro matrix solid-phase dispersion (MSPD) with electrokinetic supercharging (EKS) in capillary zone electrophoresis (CZE) has been developed for the determination of two alkaloids, lycorine and galanthamine, in complicated matrix samples. This method was comprehensively optimized in terms of the buffer condition, the leading electrolyte (LE), terminating electrolyte (TE), the sample injection in EKS preconcentration, as well as the dispersing sorbent, the sample/dispersing sorbent mass ratio, grinding time, eluting solvent in MSPD procedure. Under the optimum conditions, lycorine and galanthamine, achieved about 1500- and 1200-fold sensitivity improvement respectively when compared to the ordinary injection. A satisfactory correlation coefficient (R 2 > 0.9982) was obtained in the range of 10–500 ng/mL. The limits of detection (LODs) for lycorine and galanthamine were 6.0 ng/mL and 8.0 ng/mL, respectively. Moreover, the proposed method was successfully applied in two real samples, rat fecal samples and Bulbus Lycoridis Radiatae, to demonstrate its feasibility. Recoveries in spiked fecal and plant samples were 89.51% to 107.4%. The result showed that the new developed method possessed the great potential in analyzing trace alkaloids in complicated samples matrix.
研究领域:
分析化学
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药理学
✓ 已验证
DOI
高影响因子
Food Analytical Methods
·
2024
·
IF 2.6
Pan Xingyu,Chen Jinzi,Guo Tao,Kuang Fengjiao,Kang Zonghua,Luo Jianguang
Betel nut (Areca nut, AN) products are extensively consumed across East and South Asian countries, with Binglang being the predominant chewable AN product in China. Given the increased risk of carcinogenicity associated with alkaloid nitrogen oxides compared to the primary alkaloids in AN, this study aimed to establish a precise and sensitive method for quantitative analysis of the arecoline N-oxide (ACNO) and arecaidine N-oxide (ADNO) at three different processing stages of Binglang using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The developed method underwent comprehensive validation, evaluating key analytical parameters including selectivity, linearity, sensitivity, accuracy, precision, and stability. Notably, the method demonstrated excellent sensitivity, with the limits of detection (LOD) ranging from 0.029 to 0.135 ng/mL, while the limits of quantification (LOQ) ranging from 0.095 to 0.450 ng/mL. Subsequently, the established analytical technique was applied to analyze 15 Binglang samples at three different processing stages, providing the first evidence of the content and variability of alkaloid nitrogen oxides throughout these stages. ACNO and ADNO were detected in all samples, and their total contents ranged from 4.31 to 32.82 μg/g. The changes observed across different processing stages indicated that the roasting process at 80 ℃ resulted in the promotion of alkaloid nitrogen oxides. This analytical approach constitutes a valuable tool for the quality control and risk assessment of Binglang and can be extended to other AN products, thereby assisting in addressing health concerns associated with these products.
研究领域:
药理学
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分析化学
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食品安全
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2019
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IF 2.813
Mingxue Li,Ligai Bai,Shan Peng,Fanrong Sun,Laisen Wang,Haiyan Liu,Hongyuan Yan
A polymer-based chromatographic monolithic column was prepared via in-situ radical polymerization using tetrahydrofurfuryl methacrylate as the monomer . The homemade column was used for the separation and quantitative analysis of alkaloids, including piperine from Piper longum (fruit of Piper longum Linn .) and pepper (fruit of Piper nigrum L. ), hydroxy-α-sanshool, and hydroxy-γ-sanshool from zanthoxylum (fruit of Zanthoxylum bungeanum Maxim ), as well as caffeine from Wuyi rock tea. The chromatographic fractions were identified by mass spectrometry. Single factor test and orthogonal test were both carried out to optimize the extraction conditions. The method validation indicated that the accuracy represented by spiked recovery ranged in 98.89%–102.06%, the correlation coefficients in 0.99986–0.99999. These results show that the prepared monolithic column can be successfully used to quantitatively analyse alkaloids from the real medicinal and edible plant foods with reversed-phase mechanism, which can avoid the long analytical time using traditional packed C18 column. The present method is a simple, and inexpensive method for quantitatively analysing alkaloids from medicinal and edible plant foods, exhibiting good specificity and durability.
研究领域:
药学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2020
·
IF 3.594
Kai Hu,Tiantian Pang,Yanmei Shi,Jiamin Cheng,Yanjie Huang
In this work, a facile strategy for the preparation of magnetic porous organic framework (Ni@POFs) was proposed by the reduction of Ni ions on its skeleton in situ. The properties of the material were confirmed by X-ray diffraction, vibrating sample magnetometer, infrared spectroscopy, transmission electron microscopy and scanning electron microscopy. The prepared Ni@POFs exhibits a strong magnetism and high extraction efficiency for targeted alkaloids. All the key factors that affect the extraction/desorption efficiency of the alkaloids onto the Ni@POFs material, such as sorbent amount, extraction time, sample pH and desorption condition, were investigated with the help of response surface methodology. In combination with magnetic solid phase extraction and ultra performance liquid chromatography-tandem mass spectrometry analysis, a novel method for the quantitative analysis of alkaloids in urine samples was proposed. The limits of detection and limits of quantitation for the eight alkaloids were found to be in the range of 0.9–6.0 and 3.0–20 pg mL −1 , respectively. The recoveries of spiked urine samples were in the range of 93.5–99.2% with RSDs less than 6.9%. The proposed method was successfully applied to analyze the metabolites in patient’s urine after the oral administration of berberine.
研究领域:
分析化学
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药理学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2019
·Vol. 42
·期 24
·3646-3652
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IF 2.516
Yao Sun,Pengfei Li,Ting Wang,Liting Qin,Gege Cheng,Liqun Shen,Xingdong Yao,Shaoping Wei,Jianxin Jiang,Fuhou Lei
Alkaloids are important natural products that exhibit a wide spectrum of pharmacological activities. To efficiently separate and purify them, a rosin-based polymer-bonded silica stationary phase in high-performance liquid chromatography was synthesized via the surface radical polymerization of ethylene glycol maleic rosinate acrylate and methacrylic acid onto functionalized silica. The stationary phases, columns, optimization of chromatographic conditions for alkaloids, and thermodynamic behavior of the analytes on the column were fully studied. Under the optimized conditions, the prepared column efficiently purified natural camptothecine, caffeine, and evodiamine with the corresponding purities of 92, 96, and 97%. With this work, we have developed an efficient approach to isolate alkaloids and promoted the research on rosin-based materials in biomedicine and analytical chemistry.
研究领域:
分析化学
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天然产物化学
·
生物医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2021
·Vol. 413
·期 28
·6987-6999
·
IF 4.157
Yin Shi-Jun,Wang Xu,Jiang Hui,Lu Min,Zhou Xi,Li Li-Xian,Yang Feng-Qing
In this study, a magnetic yolk-shell structured metal-organic framework material (Fe 3 O 4 @YS-UiO-66-NH 2 ) is prepared by the directional etching of Co 2+ /peroxymonosulfate and in situ magnetization. The characteristic properties of the material were investigated by using field emission scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, X-ray powder diffraction, Fourier transform infrared spectroscopy, vibrating sample magnetometer, Brunauer-Emmett-Teller, and contact angle test. The Fe 3 O 4 @YS-UiO-66-NH 2 shows the advantages of large surface area, good magnetic property, and satisfactory stability, as well as giving high affinity to alkaloids (ALs) via hydrophilic interaction, hydrogen bonding, and π-π interaction. The results of static adsorption experiment indicate that the Fe 3 O 4 @YS-UiO-66-NH 2 possesses high adsorption capacity towards ALs and the adsorption behaviors are fitted with Langmuir adsorption isotherm model. Furthermore, a magnetic solid-phase extraction using Fe 3 O 4 @YS-UiO-66-NH 2 and HPLC method was developed for the analysis of ALs in spiked samples with the recovery of 89.6–100.8%. In addition, the proposed method was successfully applied in the pharmacokinetics study of berberine, coptisine, and palmatine in the rat. In short, the developed method might be used for high-efficient recognition and determination of ALs in plasma sample, which would also provide a new way to fabricate magnetic functionalized metal-organic framework in separation science. Graphical abstract
研究领域:
材料科学
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分析化学
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
PHYTOCHEMICAL ANALYSIS
·
2021
·Vol. 32
·期 6
·1003-1010
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IF 3.373
Xu Jia,Hanghang Zhang,Xiangfu Jiang,Yaling Lu,Wenjie Liu,Jianna Yu
Introduction Ambient pressure electrospray ionisation ion mobility spectrometry coupled to high-performance liquid chromatography (HPLC) was used to detect alkaloids from different parts of Sophora alopecuroides L. extracts. Multiplexing ion mobility spectrometry (IMS) was used to improve the signal-to-noise ratio while maintaining high resolving power for the detecting of eluents from HPLC separation. Material and methods The alkaloids profile and distribution are demonstrated by retention time-drift time two-dimensional spaces, and the contents of five major alkaloids including sophoridine, sophocarpine, cytisine, aloperine, and matrine were determined in the leaf, skin, stem, seed kernel, and seed husk using the HPLC-IMS method. This method offers extra separation ability to isomers such as matrine and sophocarpine, which can be difficult to distinguish by mass spectrometry. Results The reduced mobilities for cytisine, sophoridine, sophocarpine, matrine, and aloperine are 0.828, 0.718, 0.731, 0.725, and 0.769 cm 2 /V/s, respectively. The limits of detection are 0.553, 0.488, 0.479, 0.484, and 0.513 ug/mL. This method adds extra separation ability to HPLC to resolve co-eluted peaks and provides another qualitative parameter besides HPLC retention time.
研究领域:
植物化学
·
分析化学
✓ 已验证
DOI
高影响因子
CHROMATOGRAPHIA
·
2019
·Vol. 83
·期 2
·173-181
·
IF 1.552
Li Mingxue,Bai Ligai,Sun Fanrong,Peng Shan,Liu Haiyan,Ma Zhengyue
Abstract A four-hydrogen furfuryl-based polymer monolithic column for solid-phase extraction was prepared via in situ radical polymerization, using tetrahydrofurfuryl methacrylate as the monomer. The monolith was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy and nitrogen adsorption–desorption method, showing relatively uniform porous structure with micro-, meso- and macro-pores and a relatively high surface area of 54.99 m 2 g −1 . Online solid-phase extraction–high-performance liquid chromatography was carried out to quantitatively analyze six alkaloids, including caffeine, hydroxy-α-sanshool, hydroxy-β-sanshool, hydroxy-γ-sanshool, hydroxy-γ-isosanshool and γ-sanshool in rat plasma. The results show that the prepared polymer monolithic sorbent exhibits good clean-up ability for bio-matrix, as well as good extractive ability for the six concerning alkaloids in rat plasma. Method validation shows that the correlation coefficients of the linear regressions are higher than 0.998 and the accuracy represented by spiked recovery ranges in 94.37–100.7%, 99.52–101.1%, 98.93–100.8%, 98.36–101.6%, 99.22–101.2% and 99.86–101.4% for the six alkaloids, respectively, as well as the LOD ranges in 2.10–3.90 ng mL −1 and the LOQ in 6.35–10.14 ng mL −1 . Compared to the reference works, the present work is a simple and effective method for online extraction and simultaneous determination of six alkaloids in plasma with high accuracy and low cost. Graphic Abstract
研究领域:
分析化学
·
药理学
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）