BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 10
·e5174
·
IF 1.902
Yuan Lu,Na Li,Xiaoqin Zhu,Jie Pan,Yonglin Wang,Yanyu Lan,Yongjun Li,Aimin Wang,Jia Sun,Chunhua Liu
Polygonum orientale L . is a traditional Chinese medicine having extensive pharmacological activities including antimyocardial ischemia (MI) injury properties. Isoorientin, orientin, vitexin, quercitrin, astragalin and protocatechuic acid are the main compounds in P. orientale extract. The aim of this study was to establish an ultra-performance liquid chromatography–tandem mass spectrometry method for the determination of the content of these compounds in urine, feces and bile samples simultaneously and application of the method in a comparative excretion study in normal and MI model rats after oral administration of P. orientale extract. Chromatographic seperation was conducted on an Agilent Eclipse Plus C 18 column with the mobile phase consisting of 0.1% formic acid–acetonitrile and 0.1% formic acid–water. Negative ion multiple reaction monitoring mode was used for quantification. The six compounds had good linearity ( r ≥ 0.9921) and acceptable accuracy ranging from 10.10 to −5.82% The relative standard deviations of within-day precision and inter-day precision were <10.45 and 13.44%, respectively. The extraction recovery of the six analytes ranged from 80.31 to 101.47% and the matrix effect was 82.56–102.88%, indicating that the preparations of sample collected form urine, feces and bile were stable throughout analysis. The excretion amount of the six analytes increased in both normal and MI model rats’ urine, feces and bile in a 24 h period and became stable between 36 and 48 h after administration. The total excretion rate of six compounds was <5% in urine, feces and bile of normal and MI model rats. The excretion peak period for all compounds in MI rats was slower than that in normal rats. This excretion study provides insights for further application and research on P. orientale .
研究领域:
药理学
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分析化学
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中药学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2016
·
IF 2.687
R. Xu,H.T. Gao,F. Zhu,W.X. Cao,Y.H.M. Yan,X. Zhou,Q. Xu,W.L. Ji
This research was mainly focused on the effects of food emulsifier on the bioavailability of six priority controlling phthalate acid esters (PAEs) for the further accurate assessment of their toxic effects, using the corresponding phthalate acid monoesters (PAMEs) in rats urine as biomarkers. Glycerin monostearate was chosen as typical food emulsifier. A method was established to determine PAMEs in urine from rats either in experimental group (integrated gavaged with glycerin monostearate and PAEs) or in control group (gavaged with PAEs only), by using solid-phase extraction (SPE) coupled with ultra performance liquid chromatography tandem mass spectrometry (SPE–UPLC–MS/MS). Extraction recoveries were more than 75% for all the PAMEs; the calibration curve was linear in the range of 1.0–1000.0 ng/mL with R 2 > 0.995; the limits of detection (LOD) were 0.30 ng/mL–0.50 ng/mL. In addition, by analysing quality control (QC) urine samples in 3 days, it showed that the method was precise and accurate, for the intra-day and inter-day RSD within 16%, and the accuracy more than 82%. Internal exposure amount of all PAEs in experimental group was significantly higher than that in control group with p values of less than 0.05 except for butyl benzyl phthalates (BBP) ( P = 0.07). The bioavailability of all PAEs ranged from 5.03% to 109.35% with the presence of food emulsifiers glycerin monostearate, observably higher than that without glycerin monostearate (1.12% to 54.39%). It indicated that food emulsifiers increased the bioavailability of PAEs and may lead to potential food safety risk, which should bring awareness and be further studied.
研究领域:
毒理学
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分析化学
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食品安全
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DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2021
·Vol. 188
·期 1
·1-10
·
IF 5.833
Zheng Pimiao,Peng Tao,Wang Jianyi,Zhang Jing,Wang Zile,Zhang Yanfang,Ren Zhenhui,Wang Sihan,Jiang Haiyang
An ultrasensitive and rapid fluorescent immunoassay based on a broad-spectrum monoclonal antibody (mAb) was developed to detect pyrrolizidine alkaloids (PAs) in honey samples. First, Discovery Studio software was used to analyze and predict the target hapten, and retrorsine (RTS) was selected to react with succinic anhydride (HS) for hapten synthesization. A sensitive and broad-spectrum monoclonal antibody (mAb 13E1) was obtained for nine PAs. Then, fluorescent gold nanoclusters (AuNCs) were conjugated with mAb as a label probe and used in establishing a qualitative and quantitative lateral flow immunoassay (AuNCs-LFIA) for the determination of four PAs (retrorsine, platyphylline, senecionine, integerrimine) in honey within 14 min. The limits of detection (LOD) were 0.083 μg/kg. The recovery in spiked honey samples were 87.98–119.57%, with coefficients of variation of ≤ 11.5%. A total of 45 commercial import honey samples from nine different countries were tested through AuNCs-LFIA and UPLC-MS/MS method, and satisfactory consistency ( R 2 = 0.995) was obtained. The rates of positive samples were 55.56% (25/45), and the average concentrations of four PAs were 3.24–46.47 μg/kg. This ultrasensitive multi-PA method provides an alternative analytical tool for evaluating the human risk posed by the consumption of PA-contaminated honey. Graphical abstract
研究领域:
分析化学
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食品科学
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毒理学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Yifan Lin,Shaohua Li,Tao Chen,Yanxiang Lin,Zaixing Cheng,Lin Ni,Jin-jian Lu,Mingqing Huang
Ormosia hosiei Hemsl. et Wils. is an economical and medicinal plant , increasingly cultivated in China; however, its branches and leaves are often pruned as waste. This is the first study focused on the phytochemical profiles and antioxidant , anti- α -glucosidase, anti-tyrosinase, and anti-neuroinflammatory activities of the branches and leaves of O. hosiei . Herein, thirty-seven characteristic compounds were identified by UPLC-MS/MS and twelve were detected for the first time in O. hosiei . Twenty-seven phenolics were further quantified and significant differences in phenolic compositions between the branches and leaves of O. hosiei were observed. The ethanol extracts exhibited promising antioxidant, anti- α -glucosidase, anti-tyrosinase, and anti-neuroinflammatory effects, and the bioactivities significantly correlated with total phenolic content and twelve individual phenolics. Naringin , genistein , vitexin , vitexin-2- O -rhamnoside, syringaresinol and syringaresinol-4- O - β - D -glucopyranoside can be considered potential quality markers of O. hosiei . Our results provided solid evidence that the branches and leaves of O. hosiei deserve more attention and exploitation, considering the potential to be developed as functional foods or herbal medicines.
研究领域:
药理学
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植物化学
·
药物化学
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植物科学
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2023
·
IF 8.8
Qixun Nian,Huan Yang,Erqiong Meng,Xuerui Wan,Qiuping Zhang,Chunmin Wang,Qian Xu
This work aims to develop a widely applicable method to monitor administered AGs in various animal-derived food samples to ensure food safety. A polyvinyl alcohol electrospun nanofiber membrane (PVA NFsM) was synthesized and employed as solid-phase extraction (SPE) sorbent, in combination with UPLC-MS/MS, for the simultaneous detection of ten AGs in nine types of animal-derived food samples. PVA NFsM exhibited excellent adsorption performance for the targets (with an adsorption rate of over 91.09%), good matrix purification ability (with a reduction of 7.65%-77.47% in matrix effect after SPE), and good recyclability (can be reused 8 times). The method displayed a linear range of 0.1–25000 μg/kg and attained limits of detection for AGs were 0.03–15 μg/kg. Spiked samples demonstrated a recovery of 91.72%-100.04% with a precision of<13.66%. The practicality of the developed method was verified by testing multiple actual samples.
研究领域:
分析化学
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食品科学
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环境科学
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药物分析
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产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2026
·
IF 4.1
Zhou Xinyue,Duan Sufei,Lou Yuye,Deng Yue,Feng Shuang,Liu Jiale,Zhang Jiarui,Xi Yalin,Shi Meiyun,Yin Lei
A sensitive UPLC-MS/MS method was developed and validated for quantifying polyethylene glycol 1000 (PEG1000) in zebrafish tissues, featuring a systematic comparison of two MS acquisition strategies. Through comprehensive optimization, the ammonium adduct [M+NH 4 ] + of the representative 18-EO oligomer ( m/z 828.5) was selected as the precursor ion, achieving approximately fourfold higher signal intensity than [M+H] + . Critically, the conventional high declustering potential in-source CID approach monitoring fragment ions was outperformed by the optimized MRM method monitoring the intact ammoniated precursor, which demonstrated 2.7-fold signal enhancement and superior selectivity. The integration of micro-solid-phase extraction (μ-SPE) further improved method performance, yielding 1.5-fold signal gain and markedly reduced matrix effects compared to conventional protein precipitation. The fully validated method exhibited excellent linearity (0.5–50 μg/mL, r > 0.995), accuracy, precision, and stability. Application to zebrafish tissue distribution studies revealed pronounced organ-specific accumulation following aqueous exposure to 200 μg/mL PEG1000, with highest concentrations in intestine tissue exhibiting a time-dependent increase, followed by muscle, while muscle maintained consistently low levels. This analytical platform, synergistically combining μ-SPE cleanup and ammoniated adduct-based MRM, offers superior sensitivity over in-source CID approaches and provides a practical framework for polymer bioanalysis, yielding critical insights into the in vivo fate of PEG-based compounds. The key novelties of this work are the following: (i) the first systematic comparison between ammoniated adduct MRM and high-DP in-source CID for PEG1000 quantification; (ii) the introduction of μ-SPE for sample preparation in zebrafish tissues, achieving 1.5-fold signal enhancement; and (iii) the successful application of this platform to reveal organ-specific accumulation patterns of PEG1000. Graphical abstract
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PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2021
·Vol. 35
·期 7
·e5093
·
IF 1.902
Wei Wu,Rui Cheng,Zhenzhou Jiang,Luyong Zhang,Xin Huang
A rapid and specific UPLC–MS/MS method with a total run time of 3.5 min was developed for the determination of pravastatin, fexofenadine, rosuvastatin, and methotrexate in rat primary hepatocytes. After protein precipitation with 70% acetonitrile (containing 30% H 2 O), these four analytes were separated under gradient conditions with a mobile phase consisting of 0.03% acetic acid (v/v) and methanol at a flow rate of 0.50 mL/min. The linearity, recovery, matrix effect, accuracy, precision, and stability of the method were well validated. We evaluated drug–drug interactions based on these four compounds in freshly suspended hepatocytes. The hepatic uptake of pravastatin, fexofenadine, rosuvastatin, and methotrexate at 4°C was significantly lower than that at 37°C, and the hepatocytes were saturable with increased substrate concentration and culture time, suggesting that the rat primary hepatocyte model was successfully established. Triptolide showed a significant inhibitory effect on the hepatic uptake of these four compounds. In conclusion, this method was successfully employed for the quantification of pravastatin, fexofenadine, rosuvastatin, and methotrexate and was used to verify the rat primary hepatocyte model for Oatp1, Oatp2, Oatp4, and Oat2 transporter studies. Then, we applied this model to explore the effect of triptolide on these four transporters.
研究领域:
药理学
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分析化学
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肝脏病学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Yao Wang,Yuhan Liu,Yutong Sha,Jia Li,Luyao Han,Huili Chen,Shengdi Su,Ning Li,Xijing Chen,Di Zhao
A chiral UPLC-MS/MS method was developed and validated to determine oxiracetam enantiomers in human plasma, urine, and feces. The R-Oxiracetam and S-Oxiracetam were quantified using a CHIRALPAK ®AD3 column at 25 ℃, and the resolution was greater than 3.2. The S-Oxiracetam is the eutome r that isresponsible for the treatment of various brain damage. Isocratic elution was conducted at a flow rate of 0.9 mL/min for 6 min using the mixture of methanol and acetonitrile (methanol:acetonitrile, 15:85) containing 0.3‰ formic acid . The methods showed linearity at the range of 0.5–100 µg/mL for each oxiracetam enantiomer. A comprehensive validation process was carried out, covering aspects including linearity, selectivity, carryover, accuracy, precision, interferences, matrix effect, recovery, dilution integrity and stability in matrix and solution. The validated methods were successfully applied to quantifying R-Oxiracetam and S-Oxiracetam in human plasma, urine, and feces of 12 healthy subjects treated with either a single dose of 2 g S-Oxiracetam injection or 4 g Oxiracetam injection in a phase-I clinical trial . There was no significant difference for plasma pharmacokinetic parameters of S-Oxiracetam between the two regimens ( P＞0.05 ). The S-Oxiracetam and Oxiracetam were primarily eliminated through urine in their original form, with cumulative excretion rates of 92.16% and 85.92%, respectively, within 24 h after administration. Enantiomers interconversion was not observed in the plasma, urine, or feces. The results of this study suggest that replacing 4 g Oxiracetam injection with 2 g S-Oxiracetam injection could offer clinical benefits by lowering the dosage and mitigating potential risks, based on the pharmacokinetic characteristics.
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PubMed
高影响因子
RSC Advances
·
2018
·Vol. 8
·期 16
·8586-8595
·
IF 2.936
Wenwen Zhao,Zongyang Liu,Weiwei Guo,Kui Luo,Jie Yang,Wei Gao,Xia Wu,Xiaoqing Chen
Ilexhainanoside D (IhD) and Ilexsaponin A1 (IsA) are a pair of oleanene- and ursane-type triterpenoid saponins, which are also the main bioactive pharmaceutical ingredients of Ilex hainanensis Merr. with great potential to treat non-alcoholic fatty liver disease (NAFLD). The pharmacokinetics of four representative triterpenoids in mice were investigated in this study, which were IhD, IsA and their major metabolites 3β, 19α-dihydroxyolean-12-ene-24, 28-dioic acid (ID) and Ilexgenin A (IA). A sensitive and accurate UPLC-MS/MS method was developed and validated for the simultaneous quantitative determination of IhD, IsA, ID and IA in control and NAFLD mice plasma after oral administration of the total saponins of I. hainanensis (the contents of IhD and IsA were 41.6% and 54.4%, respectively). The results revealed that the pharmacokinetic behaviors could be changed in NAFLD mice compared with control mice. The area under the plasma drug concentration–time curve and maximum plasma concentrations of IhD and IsA were greatly decreased in the NAFLD mice. However, the main residence time of ID and IA were greatly increased in the NAFLD mice. The results revealed that this method could be used to analyze two pairs of triterpenoid isomers in biological samples.
研究领域:
药理学
·
分析化学
·
代谢
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Ruimin Lu,Yan Zhang,Daoping Zeng,Qihua Xu,Dan Wang,Peng Dai,Weijie Deng,Lin Kang,Xiaoxiao Ke,Luying Duan,Yanping Hong,Wuying Yang
An ultrasensitive indirect competitive chemiluminescence immunoassay (icCLEIA) based on monoclonal antibodies (mAb) for the effective detection of nitrofurantoin metabolite 1-aminohydantoin was developed under optimal conditions in our study. 1-aminohydantoin (AHD) was derivatized with m-formylphenoxyacetic acid (MCEP) to obtain a hapten MCEPAHD. The developed icCLEIA based on anti-MCEPAHD mAb showed high sensitivity to competing drugs 2-nitrophenyl derivative of AHD (2NPAHD) with a limit of detection (LOD) 0.04 ng/mL and a 50 % inhibitory concentration (IC 50 ) 0.27 ng/mL, and the icCLEIA had an ultra-high specificity for 2NPAHD, with little cross-reactivity with structural analogues other than parent drug nitrofurantoin. The mean recovery of AHD in fish samples was found to be 97.0 % to 118.5 %, with a coefficient of variation of less than 7.0 %. A comparison of the results of ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with those of icCLEIA demonstrated good linearity. These assay results indicated that the prepared mAb against MCEPAHD and the developed icCLEIA in our research can be used for simple, fast and sensitive detection of AHD residues in animal tissues.
研究领域:
分析化学
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免疫学
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兽医学
·
食品安全
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产品关联
DOI
高影响因子
Separations
·
2023
·Vol. 10
·期 8
·459
·
IF 2.6
Xiaoqiong Wu,Yun Lin,Xiang Zhang,Nan Ouyang,Ying Zhou
The present study employed a modified QuEChERS method to systematically analyze the presence of fifteen quinolone and seven tetracycline antibiotic residues in local animal food. Additionally, a multi-level four-factor Box–Behnken design (BBD) within the framework of response surface methodology (RSM) was utilized to evaluate the factors impacting the detection efficiency of the sample pretreatment procedure. Optimization was performed via Design Expert®10.0.3, and the factors, including the volume of the acetonitrile, the addition of formic acid, the duration of the extraction, and the addition of EDTA, were combined with experimental design until an optimal solution was reached. Finally, the sample was tested via ultra-high performance liquid chromatography-quadrupole-linear ion trap mass spectrometry (UPLC/MS/MS) in both multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan modes on a QTRAP®5500 instrument (AB SCIEX instruments, Framingham, MA, USA). The overall average recoveries from actual samples fortified with 22 antibiotics at three levels ranged from 73.8% to 98.5% based on the use of matrix-fortified calibration, with variations ranging from 5.80 to 12.4% (n= 6). The limits of detection and quantification were 0.3 μg kg−1and 1.0 μg kg−1, respectively. Lastly, the modified method was applied to practical sample analysis in the daily risk monitoring and assessment of food safety with satisfactory stability and robustness.Keywords:antibiotics residue;response surface methodology (RSM);quinolones;tetracyclines;multiple reaction monitoring (MRM)
研究领域:
分析化学
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食品科学
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药理学
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产品关联
DOI
高影响因子
Frontiers in Plant Science
·
2024
·
IF 4.1
Wang Miaomiao,Shen Qiuyu,Pang Jianyu,Mao Yu,Li Xiaofei,Tao Yanxia,Tang Wenru,Sun Ruifen,Zhou Xuhong
Objective: Carnation is a plant that holds high value in terms of its edibility, medicinal properties, and ornamental appeal. Creating no sense he aim of this study was to evaluate the antioxidant and antitumor properties of extracts derived from various parts of the carnation plant. Metabolomics technology was employed to identify the primary chemical constituents.Methods: Initially, we measured the total phenolic and total flavonoid contents in carnation roots, stems, leaves, and flowers, followed by assessing the antioxidant and anti-tumor capabilities of each component using diverse experimental methods. Subsequently, UPLC-MS/MS was employed to identify metabolites in different parts of carnation and investigate their roles in antioxidant and anti-tumor activities.Results: Mention numerical value- for better underatnding- Results of the study indicated that the methanol extract obtained from carnation flowers and roots exhibited superior antioxidant capacity compared to that from the stems and leaves. This disparity may be attributed to the abundance of polyphenols, flavonoids, and antioxidants present in the flowers, including methyl ferulate and luteolin-4’-O-glucoside. Furthermore, the significant presence of the anthraquinone compound rhein-8-O-glucoside in carnation roots may contribute to their enhanced antioxidant properties. Ten distinct compounds were isolated and recognized in carnation flowers, with Isoorientin 2”-O-rhamnoside and Kurarinone demonstrating notable antioxidant activity and binding affinity to SOD1 and SOD3, as validated through antioxidant screening and molecular docking.Conclusion: Overall, the findings from this study have expanded our knowledge of the phytochemical composition across different anatomical regions of the carnation plant, providing valuable insights for its holistic utilization.
研究领域:
植物学
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药理学
·
分析化学
·
药物化学
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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）