CHROMATOGRAPHIA
·
2012
·Vol. 75
·期 9
·499-511
·
IF 1.195
Zhang Chunhua,Wu Huiqin,Huang Xiaolan,Zhu Zhixin,Luo Huitai,Huang Fang,Lin Xiaoshan
A sensitive and selective method for simultaneous determination of 29 toxic alkaloids in human blood and 31 in urine using high-performance liquid chromatography–electrospray ionization-tandem mass spectrometry was developed and validated. The samples were diluted with 0.1 mol L −1 HCl, and the target alkaloids were purified by solid phase extraction. The separation of 31 alkaloids was carried out on a C18 column using a gradient mobile phase with 10 mmol L −1 ammonium formate in water with 0.1% formic acid and methanol at the rate of 0.25 mL min −1 . The triple-quadrupole mass spectrometer equipped with an electrospray source in the positive mode was set up in the dynamic multiple reactions monitoring mode (dynamic MRM) to detect the ion transitions of 31 alkaloids. The calibration curves were linear over a range of 0.5–400, 1–400, or 4–400 μg L −1 for target alkaloids in human blood and urine, and the correlation coefficients ( r
2 ) was higher than 0.9943. The limit of determination and limit of quantification were 0.2–1 and 0.5–4 μg L −1 for blood and urine, respectively. The only exceptions were sanguinarine and chelerythrine in human blood. All the target alkaloids were stable under the test condition. In addition, the solvent effect and reconstituted solution were investigated. The method was validated and proved to be accurate and precise over the studied concentrations and suitable for poisoning diagnosis and forensic toxicology.
研究领域:
分析化学
·
法医学
·
毒理学
✓ 已验证
产品关联
DOI
高影响因子
MOLECULES
·
2017
·Vol. 22
·期 9
·1494
·
IF 2.861
Yan Du,Zhibin Wang,Libo Wang,Mingjie Gao,Liqian Wang,Chunli Gan,Chunjuan Yang
A rapid and sensitive Ultra High Performance Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry (UHPLC-ESI-MS/MS) method was developed and validated to simultaneously determine the concentration of seven phenolic acids (syringic acid, ferulic acid, caffeic acid, vanillic acid,p-coumaric acid, 3,4-dihydroxybenzoic acid and 4-hydroxybenzoic acid) in rat plasma after oral administration ofEchinacea purpureaextract. After mixing with the internal standard (IS), butylparaben, plasma samples were prepared by liquid–liquid extraction with ethyl acetate. The separation was performed using the Agilent Eclipse Plus C18column (1.8 μm, 2.1 mm × 50 mm) with a gradient system consisting of solution A (0.1% acetic acid in water) and solution B (methanol) at a flow rate of 0.3 mL/min. The detection was accomplished by a multiple reaction monitoring (MRM) mode with electrospray ionization (ESI). The method was validated in terms of linearity, precision, accuracy, extraction recovery, matrix effect and stability. This method was successfully applied to study the pharmacokinetic properties of the seven compounds after oral administration ofEchinacea purpureaextract in rats.Keywords:Echinacea purpurea;phenolic acids;UHPLC-ESI-MS/MS;pharmacokinetics
研究领域:
分析化学
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药理学
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植物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2013
·
IF 3.334
Chunying Luo,Xixi Wang,Ge Gao,Lian Wang,Yongxin Li,Chengjun Sun
The study systematically investigated free, conjugate and total phenolics (phenolic acids and flavonoids) in leaves of 19 Chinese and one American sweetpotato cultivars grown in China. Three extraction/hydrolytic methods (direct extraction and acidic and basic hydrolysis) for sample preparation were employed to obtain different forms of phenolics. Twenty-nine phenolics were separated and identified using HPLC–DAD and HPLC–ESI–MS/MS. Three quercetin glycosides were characterised for the first time from this plant. Contents of the principal phenolics identified were determined by the HPLC–DAD procedure, which was validated in terms of linearity, precision, accuracy and limit of detection and quantification. Moreover, to the best of our knowledge, it is the first to reveal and demonstrate artifacts of esterification during acidic methanolic and ethanolic hydrolysis, and chromatographic behaviours, UV spectra and MS data of 20 hydroxycinnamic acid methyl and ethyl esters were obtained using acidic methanolic and ethanolic hydrolysis.
研究领域:
植物化学
·
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Journal of Nanomaterials
·
2021
·
IF 2.986
Yangxu Luo,Juan Du,Huadi Xiao,Ling Zheng,Xuncai Chen,Ande Ma,Qizhi Luo
Accurate identification and quantification of methamphetamine (MA) and its related substances are essential for the investigation and fair trial of drug offenses. In this study, a modified LC-ESI-MS/MS method for the simultaneous determination of MA and its isomer N-isopropylbenzylamine (N-IBA) in forensic samples was developed and validated. Optimum chromatographic separation of the target analytes was achieved on an Agilent Poroshell 120 SB-C18 column ( mm, 2.7 μm) at 40°C with isocratic elution at the flow rate of 0.40 mL/min. The mobile phase was acetonitrile and 20 mM ammonium acetate solution containing 0.1% formic acid (80 : 20, ). Positive ESI-MS/MS detection was performed in multiple reaction monitoring (MRM) mode to identify and quantify the target analytes. Method validation showed excellent linearity in the range of 0.51 ng/mL~51 ng/mL for MA and N-IBA. The low limit of detection (LLOD) and low limit of quantification (LLOQ) reached 0.1 ng/mL and 0.3 ng/mL for both analytes. The method showed a satisfactory accuracy with an inter- and intraday-relative error (RE) <20%, and a precision of inter- and intraday relative standard deviation (RSD) less than 15%. The validated method was successfully applied in real forensic samples and resulted in the detection of MA and N-IBA in 8 suspected samples in drug cases that only deemed MA positive using our previous routine screening procedure, which avoided the misidentification of N-IBA as MA.
研究领域:
分析化学
·
法医学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Jie Wang,Yuan-Yuan Zhang,Dan Liu,Chen-Chun Zhong,Ya-Hui Hu,Fei Zhao,Hong-Li Guo,Feng Chen
The balance of oxalic acid in the body is intricately regulated. Importantly, elevated levels of oxalic acid in urine or blood have been linked to the progression of various diseases. There is strong interest in developing efficient methods to quantify oxalic acid in various bio-matrices like urine. However, due to its small molecular weight, high polarity, acidic nature, and endogenous properties, establishing an analysis method based on liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) for oxalic acid presents significant challenges, and such analysis methods that meet clinical needs are not widely available. Faced with the aforementioned challenging issues, in this study, we have discovered innovative strategies to improve the ionization, chromatographic separation, and enrichment of oxalic acid and its internal standard, leading to the successful LC-MS/MS method development and clinical application of the analysis method. These include: (1) simultaneous use of two low concentrations of electrolytes (NH 3 ·H 2 O and NH 4 Ac) in the mobile phase; (2) alkalinization of urine; (3) addition of 0.3 % NH 3 ·H 2 O to the internal standard oxalic acid-1,2- 13 C solution; (4) selection of ultrapure water (UPW) as an alternative matrix; (5) urine sample processing using an easy-to-use protein precipitation method. These measures have created a relatively homogeneous alkaline environment, addressing the issues in the ionization, chromatographic separation, and enrichment of oxalic acid and its internal standard. Of note, chromatographic separation of oxalic acid and oxalic acid-1,2- 13 C was achieved on the Waters Symmetry C18 column (4.6 mm × 50 mm, 3.5 μm) with an isocratic elution at a flow rate of 0.40 mL/min. The target analyte was completely separated by elution with 30 % acetonitrile containing 0.01 % NH 3 ·H 2 O and 1 mM NH 4 Ac for 3 min, without any endogenous interference. The method showed good linearity over the 0.020–50.0 μg/mL concentration range with a correlation coefficient r 2 = 0.9998. The intra-assay and inter-run precision and accuracy, recovery, and stability of the method were all within the acceptable parameters. Collectively, this study developed and validated a simple, fast, and sensitive LC-ESI-MS/MS method that did not require complex derivatization, acidification, large-volume sample consumption. Moreover, this method was successfully applied for routine urinary oxalic acid detection in children with kidney disease, providing valuable information for clinicians.
研究领域:
临床医学
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分析化学
·
肾脏病学
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
Shenxiong Chen,Yi Yuan,Fan Zhang,Shiye Lin,Pengren Zou,Mohamed A. Farag,Jesus Simal-Gandara,Hui Cao,Jianbo Xiao
Grape seed wastes are a rich source of bioactive polyphenols. This study compares the recovery efficiency of traditional maceration extraction (ME) with modern extraction techniques (ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), and accelerated solvent extraction (ASE)), revealing the selective extraction of polyphenolic compounds by different methods. UPLC-ESI-MS/MS analysis was used to identify and quantify 24 polyphenols. ASE showed the highest efficiency for phenolic acids (e.g., gallic acid, 231.75 μg/g) and proanthocyanidins (e.g., procyanidin B1, 126.18 μg/g), while MAE was optimal for flavonoids recovery (e.g., myricetin, 41.52 μg/g). Multivariate chemometric analysis revealed co-extraction patterns among structurally related compounds (e.g., flavan-3-ols with galloylated derivatives), linking extraction parameters to the selectivity of polyphenols. Integrating UPLC-ESI-MS/MS profiling of 24 polyphenols, we suggest that MAE/ASE is most suitable for antioxidant-rich nutraceuticals, while ME is optimal for thermally labile pharmaceuticals. This study provides practical strategies for the sustainable utilization of grape seed by-products, offering industry-specific solutions to reduce waste and improve the recovery of bioactive compounds.
研究领域:
食品科学
·
分析化学
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植物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2018
·Vol. 23
·期 4
·714
·
IF 3.098
Weijuan Du,Lisha Jin,Liping Li,Wei Wang,Su Zeng,Huidi Jiang,Hui Zhou
The tuber ofCorydalis yanhusuois a famous traditional Chinese medicine and found to have potent pharmacological effects, such as antinociceptive, antitumor, antibacterial, anti-inflammatory, and anti-depressive activities. Although there are several methods to be developed for the analysis and detection of the bioactive ingredients’ alkaloids, so far, only few prominent alkaloids could be quantified, and in vitro and in vivo changes of comprehensive alkaloids after oral administration are still little known. In this study, we first developed a simple and sensitive high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) method to quantify the comprehensive alkaloids of extracts ofC. yanhusuoin mouse plasma, using nitidine chloride as an internal standard. As results, at least fourteen alkaloids, including an aporphine (oxoglaucine), a protopine (protopine), five tertiary alkaloids (corydaline, tetrahydroberberine, tetrahydropalmatine, tetrahydrocolumbamine, and tetrahydrocoptisine) and seven quaternary alkaloids (columbamine, palmatine, berberine, epiberberine, coptisine, jatrorrhizine, and dehydrocorydaline) could be well quantified simultaneously in mouse plasma. The lower limits of quantification were greater than, or equal to, 0.67 ng/mL, and the average matrix effects ranged from 96.4% to 114.3%. The mean extraction recoveries of quality control samples were over 71.40%, and the precision and accuracy were within the acceptable limits. All the analytes were shown to be stable under different storage conditions. Then the established method was successfully applied to investigate the pharmacokinetics of these alkaloids after oral administration of the extract ofCorydalis yanhusuoin mice. To the best of our knowledge, this is the first document to report the comprehensive and simultaneous analyses of alkaloids ofC. yanhusuoin mouse plasma. It was efficient and useful for comprehensive pharmacokinetic and metabolomic analyses of these complex alkaloids after drug administration.Keywords:alkaloids;Corydalis yanhusuoextract;pharmacokinetics;HPLC-ESI-MS/MS;oxoglaucine
研究领域:
中药学
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分析化学
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药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2023
·
IF 8.8
Jinlong Wu,Changwen Chen,Yong Li,Ke Cao,Xinwei Wang,Weichao Fang,Gengrui Zhu,Lirong Wang
The characterization of peach metabolites and carotenoids during canning and storage remains unclear. The present study identified 658 metabolites and 40 carotenoids in peach fruits throughout the canning and storage using ESI-MS/MS and APCI-MS/MS based metabolome approach. A total of 282 differentially accumulated metabolites were found, mainly including 78 phenolic acids, 74 lipids, 61 flavonoids. Five esterified carotenoids (rubixanthin palmitate, β-cryptoxanthin oleate, β-cryptoxanthin laurate, β-cryptoxanthin palmitate, and β-cryptoxanthin myristate) were the main peach carotenoids, with a proportion of approximately 90%, while free carotenoids accounted for 4.22–5.95% during the entire processing period. Moreover, the total carotenoid loss rates for canning and storage were 56.67% and 46.55%, respectively. Compared to the loss of free carotenoids, esterified carotenoids were more stable during storage, while canning led to a greater loss of esterified carotenoids. The results provided new insights into the maintenance of health-related phytochemicals from canning processes.
研究领域:
食品科学
·
代谢组学
·
农学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2024
·
IF 6
Wen Ouyang,Jingming Ning,Xizhe Zhu,Yongwen Jiang,Jinjin Wang,Haibo Yuan,Jinjie Hua
Fixation is crucial for green tea quality; previous studies were conducted on finished teas and focused on the volatile metabolites of green tea. However, non-volatile metabolites’ (NVMs) evolution and formation mechanisms during fixation remain unclear. Here, fixated tea samples were collected at seven different time points during the green tea fixation stage, the dynamic changes and formation mechanisms of NVMs investigated via ultra-performance liquid chromatography-tandem mass spectrometry and enzymatic activity analyses. The results showed that fixation contained enzymatic activity thermal and non-enzymatic thermal stages. Moreover, 1196 NVMs (10 classes) were detected, and significant NVM variations were observed during the "enzymatic activity thermal" fixation stages, with increasing trends in lipids and amino acids, except alkaloids. Furthermore, 160 common differential NVMs were identified. KEGG analysis revealed that unsaturated fatty acid, linoleic acid phenylpropanoid, and flavonoid metabolism pathways were essential during fixation and influenced green tea aroma, taste, and color formation. These results provide a theoretical basis to regulate green tea fixation technology and enrich the chemical theory of green tea processing.
研究领域:
食品科学
·
分析化学
·
植物代谢
·
茶叶加工
✓ 已验证
产品关联
DOI
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 8
·e4256
·
IF 1.688
Fugeng Zhang,Xiaoli Qiao,Hui Lu,Shaoqiang Zhang,Wuxun Du,Xuefeng Xiao
Yiqifumai Injection is a lyophilized powder preparation widely used to treat coronary heart disease. However, its in vivo bioactive components and pharmacokinetic behavior remain unknown. Therefore a sensitive and specific LC–MS/MS was developed and validated for the simultaneous quantification of eight saponins and four lignans in beagle dog plasma. The plasma samples were pretreated by protein precipitation with methanol–acetonitrile (1:1, v /v). Chromatographic separation of all the 12 analytes and estazolam (internal standard, IS) was successfully accomplished on an Ultimate® XB-C 8 column (100 × 2.1 mm, 3 μm) with a gradient elution system. The total running time was 8 min with a flow rate of 0.40 mL/min. Acquisition of mass spectrometric data was performed via positive electrospray ionization in multiple reaction monitoring mode. The assay was fully validated in terms of selectivity, linear range, lower limit of quantitation, precision, accuracy, matrix effect, recovery and stability. This validated method was successfully applied to the pharmacokinetics of 12 bioactive components after intravenous administration of Yiqifumai Injection to beagle dogs at a dose of 0.541 g/kg.
研究领域:
药理学
·
分析化学
·
兽医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Food Science and Human Wellness
·
2023
·
IF 7
Hui Zou,Tingting Ben,Ping Wu,Geoffrey I.N. Waterhouse,Yilun Chen
This novel study identifies the effective anti-inflammatory phenolic compounds in dandelion and provides mechanistic insights into their interactions with receptor proteins (toll‐like receptor 4, TLR4; co‐receptor myeloid differentiation protein-2, MD-2) using UHPLC-ESI-MS/MS, lipopolysaccharide (LPS)-stimulated THP-1 cell line, fluorescence quenching and anisotropy, molecular docking (single ligand and multi-ligand docking) and molecular dynamics simulation. A 50 % aqueous methanol extract had a greater anti-inflammatory effect and higher chicoric acid content, compared with the 100 % water and 100 % methanol extracts. Chicoric acid, chlorogenic acid, methylophiopogonone A, caffeic acid, gallic acid monohydrate and 4'- O -demethylbroussonin A had relatively high binding energies and contents in all extracts. Chicoric acid competed with chlorogenic acid, 4'- O -demethylbroussonin A and quercetin for MD-2. Among dandelion’s phenolics, chicoric acid most effectively hindered TLR4-MD-2 complex formation, with a quenching constant of 0.62 × 10 6 L/mol for MD-2 or TLR4 at 320 K, and binding energies of –6.87 and –5.97 kcal/mol, respectively, for MD-2 and TLR4.
研究领域:
药理学
·
生物化学
·
分子生物学
·
分析化学
·
免疫学
✓ 已验证
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Fábio de Souza Barbosa,Leonardo Capra Pezzi,Marisa Tsao,Sandra Manoela Dias Macedo,Tiago Franco de Oliveira,Elfrides E.S. Schapoval,Andreas S.L. Mendez
An ESI-MS/MS method through direct infusion was validated for quantitative analysis of meropenem powder for injection. The validation parameters were established in a rapid analysis of 30 s. Drug stability was studied through the submission to stress testing, resulting on four degradation products. Under hydrolytic conditions, in acid, neutral and alkaline media, the major degradation product was formed through the cleavage of the β-lactam ring. Oxidation of the drug using H 2 O 2 (3%) showed the formation of two degradation products from a decarboxylation reaction and N-oxide formation. Under high humidity conditions, there was detected a dimer product. The stability of meropenem after reconstitution was studied in conditions that simulate its clinical use. In samples reconstituted and diluted in infusion fluids, an extensive degradation was observed. At room temperature meropenem maintained its content > 90% for up to 4 h when prepared in 5% glucose and for up to 12 h when prepared in 0.9% NaCl. Through ESI-MS/MS analyzes it was observed a degradation product formed by β-lactam ring cleavage, detected in all conditions studied. It was also identified a degradation product formed only in 5% glucose, generated by the hydrolysis of β-lactam followed by the attachment of a glucose molecule to the nitrogen of the pyrrolidine ring. In general, all the results obtained in the stability studies contribute to the knowledge about this antibiotic and future candidates of this class.
研究领域:
药学
·
分析化学
·
药物代谢
✓ 已验证
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）