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
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法医学
·
毒理学
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产品关联
DOI
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
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食品科学
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分析化学
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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
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DOI
PubMed
高影响因子
Frontiers in Plant Science
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2017
·
IF 4.291
Chen Guilin,Guo Mingquan
Topoisomerase I (Topo I) catalyzes topological interconversion of duplex DNA during DNA replication and transcription, and has been deemed as important antineoplastic targets. In this study, the fraction R.d-60 from ethyl acetate extracts of Rhamnus davurica showed higher inhibitory rates against SGC-7901 and HT-29 compared with the R.d-30 fraction in vitro. However, the specific active components of R.d-60 fraction remain elusive. To this end, a method based on bio-affinity ultrafiltration and high performance liquid chromatography/electrospray mass spectrometry (HPLC- ESI-MS/MS) was developed to rapidly screen and identify the Topo I inhibitors in this fraction. The enrichment factors (EFs) were calculated to evaluate the binding affinities between the bioactive constituents and Topo I. As a result, eight ligands were identified and six of which with higher EFs showed more potential antitumor activity. Furthermore, antiproliferative assays in vitro (IC50 values) with two representative candidates (apigenin, quercetin) against SGC-7901, HT-29 and Hep G2 cells were conducted and further validated. Finally, the structure-activity relationships revealed that flavones contain a C2-C3 double bond of C ring exhibited higher bio-affinities to Topo I than those without it. This integrated method combining Topo I ultrafiltration with HPLC-MS/MS proved to be very efficient in rapid screening and identification of potential Topo I inhibitors from the complex extracts of medicinal plants, and could be further explored as a valuable high-throughput screening platform in the early drug discovery stage.
研究领域:
药理学
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分析化学
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肿瘤学
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DOI
PubMed
高影响因子
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2017
·
IF 3.154
Xiaoyan Liao,Fangli Hu,Zilin Chen
Information on the chemical composition of Osmanthus fragrans fruits is still limited because there are many compounds present in low concentrations in the plant. In this work, the bioactive components in O. fragrans fruit extract were investigated by a new high-performance liquid chromatography electrospray ionization tandem mass spectrometry method, which allows sensitive analysis both in identification and quantitation. A total of 28 compounds were tentatively identified, and 16 components were discovered in O. fragrans fruits for the first time. The validated quantitative methods for the determination of the bioactive components were subsequently applied to analyze batches of O. fragrans fruits from different cultivars, which is beneficial for the comprehensive utilization of O. fragrans fruits.
研究领域:
分析化学
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植物化学
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食品科学
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产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2022
·Vol. 14
·期 25
·2531-2540
·
IF 3.532
Wenjing Li,Maoyu Cao,Pengxiang Ge,Xiaoyu Fu,Jiajie Tang,Mindong Chen
Organosulfates (OSs) derived from the oxidation of biogenic volatile organic compounds (BVOCs) in the presence of anthropogenic sulfate aerosols are the important tracers of secondary organic aerosols (SOAs). In order to better understand the concentration of pinene-nitrooxy organosulfates (pNOSs) in Nanjing, a sensitive high-performance liquid chromatography-electron spray ionization spectrum/mass spectrum (HPLC-ESI-MS/MS) to determine pNOSs in PM2.5 has been developed and validated in this study. Firstly, Hypersil Gold C18 (Thermo Scientific, San Jose, USA) was selected to separate pinene-derived nitrooxy organosulfates (pNOSs) based on their polarity. Three kinds of pNOSs were detected in the full scan mode (MS) with an ESI source under the negative mode. Secondly, three isomers of pNOSs with fragment ions m/z 220, 151, and 142 were identified based on the MS/MS maps. At least two pairs of transfer ions should be selected as identification and quantification ions according to the optimization results of target compounds. For example, to determine pNOSs, these transfer ions of m/z 294 → 247, m/z 294 → 231, m/z 294 → 220, m/z 294 → 142, m/z 294 → 151, m/z 294 → 96, m/z 294 → 80 were selected as quantification and identification ions. Finally, the influence of scan mode on pNOS detection was evaluated, and the results showed that pNOSs were most sensitive in the SRM (selected reaction monitor) scan mode. Therefore, the SRM scan mode was chosen to detect pNOSs. We applied this method to analyze year-round PM2.5 (PM2.5 is fine particulate matter, which refers to particulate matter in ambient air with an aerodynamic equivalent diameter of less than or equal to 2.5 microns) samples in Nanjing. The average concentration of all the three kinds of pNOSs was 69.95 ng m−3. The results showed that the average concentration of pNOSs was high in spring (92.94 ng m−3) and summer (90.57 ng m−3), and lowest in winter (30.03 ng m−3).
研究领域:
大气化学
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环境科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2026
·
IF 1.1
Jianwei Wang,Xin Tian,Jun Zhang
Polyoxyethylene alkyl ether carboxylic acid (AEC) is a high-performance surfactant widely used in personal care and industrial applications. Existing analytical frameworks often struggle with low sensitivity and the inability to simultaneously quantify active ingredients alongside residual raw materials. This study describes the development and validation of an HPLC-ESI-MS method for the comprehensive characterization of AEC products. Chromatographic separation was achieved on an XBridge® C18 column using a mobile phase consisting of methanol and 25 mmol/L ammonium formate (containing 0.2% formic acid) (80:20, v/v). The method enables the accurate quantification of residual AEO and the semi-quantitative estimation of the key byproduct polyethylene glycol ether carboxylic acid (PEG-CH2COOH). For C12-14 AEO and PEG-CH2COOH, the LODs were 0.2 and 0.5 μg/mL, and the LOQs were 0.6 and 1.5 μg/mL, respectively. Excellent linearity was observed (r ≥ 0.998), with mean recoveries ranging from 95.9% to 106.0%. Furthermore, mass spectrometric characterization facilitated the structural elucidation of PEG-CH2COOH. Based on these analytical findings, potential formation pathways involve the covalent incorporation of carboxymethyl groups through the oxidation or carboxymethylation of PEG terminal hydroxyl groups. This method provides a critical analytical tool for the quality control, safety assessment, and formulation optimization of AEC products.
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DOI
高影响因子
STEROIDS
·
2015
·
IF 2.639
Xinxin Zhang,Zengjun Guo,Jing Li,Yoichiro Ito,Wenji Sun
A specific high performance liquid chromatography tandem mass spectrometry (HPLC–MS/MS method) was established for determining the concentration of protodioscin (PG) in rat plasma after intragastric administration of its standard form. Ginsenoside Rb 1 was selected as the internal standard (IS). The plasma sample was prepared using one-step deproteinization procedure by adding three parts of acetonitrile to precipitate proteins. The chromatographic separation was accomplished on an Inersil ODS-3 C 18 column (250 × 4.6 mm, 5 μm) with a mobile phase composed with acetonitrile and water containing 0.1% formic acid under a gradient elution mode at a flow rate of 1 mL min −1 . A 3:1 portion of the eluent after a microsplit was detected on a triple quadrupole tandem mass spectrometer coupled with electrospray ionization (ESI) in positive ion and multiple reaction monitoring (MRM) scanning modes. The mass transitions were selected as 888.1 → 1050.2 for PG and 948.2 → 1110.3 for IS, respectively. After careful validation, the plasma samples were always stable under different storage conditions. These analytical results rendered sensitive, selective, and reliable values by this established method which displayed high accuracy, adequate extracted recoveries, and almost negligible matrix effects. This method was applied to the pharmacokinetic studies on PG level in the rat plasma and its pharmacokinetic effect. The results of our studies suggest that the present method may be a useful tool for further clinical study of PG.
研究领域:
分析化学
·
药物代谢
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生物医学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF MOLECULAR LIQUIDS
·
2022
·
IF 6.633
Hang Li,Qingsheng Zhao,Senlin Chang,Liwei Wang,Bing Zhao
Industrial hemp is an important economic crop. The extract of its leaves is well-known as cannabidiol full-spectrum oil (CFSO) and has great application potential. But the chemical composition of CFSO is still not clear, which limits its efficient application. Therefore, this work aimed to explore the phytochemical profile and composition-activity relationship of CFSO. The results showed that a total of 12 cannabinoids were identified by HPLC-ESI-MS and they were CBD-C 1 , CBGVA, CBGA, CBGV, CBDVA, CBG, CBDV, CBDA, CBD, CBD-C 4 , CBN, and CBT. CBD (559.3 mg/g) was the most abundant component, followed by CBDV (302.4 mg/g) and CBN (31.7 mg/g). Besides, the content of CBDV, CBD, and CBN of different polar extracts increased with the rise of ethanol concentration. The TPC and TFC of the extracts also increased with the rise of ethanol concentration. The extract of 90 % EtOH had the highest TPC (949.21 ± 2.37 mg GAE/g extract) and TFC (267.05 ± 1.21 mg RE/g extract) while the extract of 0 % EtOH displayed the lowest TPC (244.89 ± 2.13 mg GAE/g extract) and TFC (46.26 ± 0.85 mg RE/g extract). Furthermore, as ethanol concentration increased, the cytotoxicity, antioxidant, and antibacterial activities of the extracts had a significant increasing trend. And the correlation analysis demonstrated that the antioxidant activity and cytotoxicity of the extracts were closely related with the phenolic compounds and flavonoids, especially cannabinoids. These findings could provide data support for the application of CFSO.
研究领域:
药理学
·
化学
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植物科学
·
分析化学
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产品关联
DOI
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2024
·
IF 7.7
Shuangyu Shao,Xiali Si,Yingtao Zhang,Jun Li,Pengfei Tu,Qingying Zhang
Quality analysis of edible mushrooms based on polysaccharides is generally difficult due to their complicated structures and hard separation. Here, multiple fingerprint analysis of polysaccharides based on chromatographic and spectrometric techniques were developed, and then applied in comparative analysis of Auricularia heimuer (AH), Auricularia cornea (AC), Auricularia cornea ʻYu Muerʼ (ACY) and Tremella fuciformis (TF). Firstly, polysaccharides were obtained with the molecular weights between 1.783 × 10 6 and 6.774 × 10 6 Da. Then, complete hydrolysis by TFA and enzyme digestion by cellulase were employed and subsequently analyzed by HPLC-UV, GC–MS, HILIC-HPLC-ELSD and HILIC-HPLC-ESI − -HCD-MS/MS, and ATR-FT-IR were used to characterize the functional groups of intact polysaccharides. By chemometric analysis, differential markers of d -xyl, l -fuc, l -arb, d -glc, disaccharide and hexasaccharide were selected, and AC and ACY were proved to be same species from the viewpoint of polysaccharides firstly. Furthermore, the structures of oligomers with DPs of 2–8 and →4)- β - d -Glc p -(1→ unit with different contents were inferred by combinatory analysis of ESI − -MS/MS, glycosidic linkage, monosaccharide compositions and functional groups. In conclusion, the combinatory method of multiple fingerprint and pattern recognition is powerful not only for structural elucidation of polysaccharides, but also for quality analysis and species differentiation of edible mushrooms from the perspective of biological polysaccharides.
研究领域:
食品科学
·
分析化学
·
真菌学
·
生物化学
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产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）