Journal of Pharmaceutical Analysis
·
2017
·
IF 0
Jing Zeng,Hua lin Cai,Zhi ping Jiang,Qing Wang,Yan Zhu,Ping Xu,Xie lan Zhao
A sensitive, rapid, simple and economical ultra-performance liquid chromatography–tandem mass spectrometric method (UPLC–MS/MS) was developed and validated for simultaneous determination of imatinib, dasatinib and nilotinib in human plasma using gliquidone as internal standard (IS). Liquid-liquid extraction method with ethyl acetate was used for sample pre-treatment. The separation was performed on an Xtimate Phenyl column using isocratic mobile phase consisting of A (aqueous phase: 0.15% formic acid and 0.05% ammonium acetate) and B (organic phase: acetonitrile) (A:B=40:60, v/v). The flow rate was 0.25 mL/min and the total run time was 6 min. The multiple reaction monitoring (MRM) transitions, m/z 494.5→394.5 for imatinib, 488.7→401.5 for dasatinib, 530.7→289.5 for nilotinib and 528.5→403.4 for IS, were chosen to achieve high selectivity in the simultaneous analyses. The method exhibited great improvement in sensitivity and good linearity over the concentration range of 2.6–5250.0 ng/mL for imatinib, 2.0–490.0 ng/mL for dasatinib, and 2.4–4700.0 ng/mL for nilotinib. The method showed acceptable results on sensitivity, specificity, recovery, precision, accuracy and stability tests. This UPLC–MS/MS assay was successfully used for human plasma samples analysis and no significant differences were found in imatinib steady-state trough concentrations among the SLC22A5 −1889T>C or SLCO1B3 699G>A genotypes ( P >0.05). This validated method can provide support for clinical therapeutic drug monitoring and pharmacokinetic investigations of these three tyrosine kinase inhibitors (TKIs).
研究领域:
药理学
·
临床医学
·
分析化学
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DOI
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2026
·
IF 5.3
Simeng Shao,Yi Wu,Peng Yu,Xilin Wan,Hongmei Yang
Panax ginseng is widely utilized as a functional food ingredient. The steaming process is a critical treatment that profoundly alters the metabolic profiles and enhances the therapeutic properties of Panax ginseng . This study characterized ginsenosides, saccharides, and amino acids in eight ginseng samples using ultra-performance liquid chromatography-mass spectrometry (UPLC-MS) and multivariate data analysis. A total of 224 ginsenosides were identified, with 128 compounds exclusively detected in black ginseng (BG). Quantitative analysis of 49 metabolites showed that BG was enriched in rare ginsenosides (e.g., Rg3, Rg5, and Rk1) and monosaccharides (glucose and fructose) but had lower levels of basic amino acids, particularly arginine. Partial least-squares discriminant analysis (PLS-DA) identified 10 key discriminative markers distinguishing BG from other varieties. Furthermore, desorption electrospray ionization mass spectrometry imaging (DESI-MSI) visualized the spatial distribution of these markers, revealing their preferential accumulation in the cambium and phloem tissues. These findings provide comprehensive insights into the phytochemical transformation of ginseng during mild thermal processing, facilitating the development of BG as a functional food ingredient and supporting quality control in the food industry.
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高影响因子
APPLIED BIOCHEMISTRY AND BIOTECHNOLOGY
·
2025
·
IF 3.3
Li Xudong,Cui Mingxuan,Zhu Lijie,Zhang Haoqian,Guan Yunhui,Song Xiangjia,Zhao MengLin,Li Zhiguo,Liao Fei,Shi Liqiang,Zhao Ningning
Portulaca oleracea L. (PL) has significant clinical efficacy in treating ulcerative colitis (UC), which significantly affects patients’ daily life. However, the absorption and metabolism of PL in vivo remain unclear due to the difficulty in detecting organic acids. This study focused on analyzing the pharmacogenetic composition of PL extract in 24 rats ( n = 6) and its targeted network pharmacology. Using UPLC MS with derivatization techniques, plasma, and faeces were collected from healthy and UC rats gavaged with PL extracts. Subsequently, in vitro derivatization of the above biological samples and PL extracts was performed before and after derivatization to qualitatively analyze to ensure biosafety. A total of 61 active constituents and 21 constituents in vivo were detected. After derivatization, the sensitivity for detecting non-acid compositions increased in the negative mode, and the sensitivity for detecting acids also increased in the positive mode. For plasma and intestinal analysis, the detective sensitivity of organic acid was effectively increased for 1–3 times, and healthy rats with PL were detected with higher levels of the active constituents than that of UC rats with PL. Combined with the pharmacological analysis of the targeting network, it might act through the hypoxia-inducible factor-1 (HIF-1) signaling pathway and phosphatidylinositol 3-kinase (PI3K-Akt) signaling pathway. However, individual differences in the samples may limit the generalizability of the results, and further validation with larger sample sizes is needed. This study not only provides a scientific basis for the material basis of the medicinal effects but also provides new ideas and methods for the study of traditional Chinese medicines. Graphical
研究领域:
药理学
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分析化学
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中医药学
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代谢组学
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炎症性肠病研究
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Hualu Wu,Saili Xie,Xiaohai Chen,Hailun Xia,Yuxin Shen,Ren-ai Xu,Wei Tan,Ruanjuan Zhan
Fuzuloparib is a novel orally bioactive poly-ADP-ribose polymerase inhibitor (PARPi), which was approved by the Chinese Regulatory Agency (CRA) in 2020 for the treatment of platinum-sensitive recurrent ovarian, fallopian tube, and primary peritoneal cancers. This study firstly presents a rapid and accurate ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for analyzing the levels of fuzuloparib and its major metabolite (SHR165202), and to investigate drug-drug interaction between fuzuloparib and curcumin in vitro and in vivo studies. After protein precipitation with acetonitrile, mobile phase consisted of acetonitrile and 0.1 % formic acid with a gradient elution was used to successfully separate fuzuloparib, SHR165202 and talazoparib (internal standard, IS). The results indicated that fuzuloparib and SHR165202 had good linearity over the calibration range of 2–50 ng/mL and 1–20 ng/mL, respectively. The precision, accuracy, stability, matrix effect, and extraction recovery required for methodological validation all complied with the requirements of the Bioanalytical Method Validation Guidelines. In vitro microsome incubation experiments, curcumin exhibited inhibitory effect on fuzuloparib in both rat liver microsomes (RLM) and human liver microsomes (HLM) with half-maximal inhibitory concentration (IC 50 ) value of 10.54 μM and 47.64 μM, respectively, and the corresponding mechanism was non-competitive. Furthermore, the inhibitory mechanism of curcumin on fuzuloparib was validated through molecular docking. In pharmacokinetic experiments in rats, curcumin significantly altered the plasma exposure of fuzuloparib, resulting in significant increases in AUC (0-t) and C max of fuzuloparib and a significant decrease in CL z/F . Moreover, the metabolite SHR165202 showed significant increases in AUC (0-t) , AUC (0-∞) , T max and C max and a significant decrease in CL z/F . This further supports the notion that curcumin could inhibit the metabolism of fuzuloparib. Therefore, when co-administering fuzuloparib and curcumin in clinic, it is recommended to monitor plasma levels of fuzuloparib and pay close attention to adverse effects. If necessary, the dose of fuzuloparib needs to be reduced.
研究领域:
药理学
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分析化学
·
肿瘤学
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DOI
PubMed
高影响因子
MOLECULES
·
2025
·Vol. 30
·期 4
·852
·
IF 4.6
Qiqi Jin,Qianwen Xu,Zhiyong Zhao,Wenshuai Si,Bing Bai,Lei Chen,Changyan Zhou
This study presents a method for the simultaneous determination of six acidic herbicides and their metabolites in various matrices, including fruits, vegetables, grains, and edible oils. The method employs acidified acetonitrile extraction combined with dispersive solid-phase extraction cleanup (dSPE) using MgSO4, Florisil, and Graphitized carbon black (GCB). The analysis was performed by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) with electrospray ionization (ESI) in both positive and negative modes using multiple reaction monitoring (MRM). The mass concentrations of six herbicide pesticides and their metabolites were predominantly within the range of 0.0005~0.050 mg/L and exhibited strong linear relationships with the corresponding peak area, with the coefficient of determination (R2) exceeding 0.993. The limits of detection (LOD) for the method ranged from 0.0001 to 0.008 mg/kg. The recovery rates of adding recovery experiments to cabbage, chives, pear, wheat flour, and soybean oil were 69.8~120%, and the relative standard deviation (RSD) was 0.6~19.5%. The results indicate that this method is efficient and fast, and can be used for the detection of compounds in various actual matrices.
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PubMed
高影响因子
Food Science and Technology
·
2021
·
IF 1.718
WU Chunying,WANG Shuyu,TAO Ou,ZHAN Xueyan
This paper provided a method for determining the potential quality markers in Xiao'er Xiaoji Zhike oral liquid (XXZOL) based on the concordant tastes of compounds with their respective originated Chinese medicinal pieces. UPLC-Q-Exactive-Orbitrap-MS technology was used to identify the main chemical constituents in XXZOL. The electronic tongue collected the electronic responses of the sour, bitter, sweet, pungent, and salty sample solutions, and the discriminant factor analysis (DFA) model was established to recognize the taste characteristics of 23 liquid samples. Fifteen high content ingredients in XXZOL were identified by UPLC-MS, and the established DFA model recognized their respective tastes. The accurate recognition rate of the DFA model was 73.33%, the false rate was 6.67%, and the unrecognized rate was 20%. The concordance rate of their authentic tastes with the tastes of their respective originated Chinese medicinal pieces was 78.57%. Trigonelline, malic acid, citric acid, and caffeic acid were the potential sour material bases of XXZOL. Mannitol was the potential sweet material basis of XXZOL. L-phenylalanine, sinapine, forsythoside I, pinoresinol-4-O-β-D-glucopyranoside, naringin, and neohesperidin were the potential bitter material bases of XXZOL. So the above 11 main compounds were the potential quality markers of XXZOL.
研究领域:
药物分析
·
中药学
·
分析化学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2015
·
IF 2.729
Min Liao,Xiao Chen,Jiefeng Chen,Mengping Liu,Junyi Wang,Zuanguang Chen,Zhiyong Xie,Meicun Yao
An original and sensitive ultraperformance liquid chromatography–tandem mass spectrometric (UPLC–MS/MS) method for the determination of pseudoprotodioscin (PPD) in rat plasma was developed and validated. Digitoxin was applied as an internal standard. Plasma samples were processed by acetonitrile-mediated plasma protein precipitation and chromatographed using a step gradient program on a C18 column (2.1 × 50 mm i.d., 1.7 μm). The mobile phase was comprised of acetonitrile and 0.1 mmol L −1 aqueous lithium acetate mixed with 0.03% formic acid at the flow rate of 0.2 mL min −1 . Multiple reaction monitoring (MRM) transitions were performed for detection and lithium adduct ions were employed with a significant improvement of the response of the analytes in electrospray positive ionization mode. The concentration range of calibration curve was linear over the range 2–5000 ng mL −1 . The intra- and inter-day precisions were all less than 11.5% and accuracies were within the range of 94.1–103.5%, and the analytes exhibited no severe matrix effect. The validated method was successfully applied in the pharmacokinetics of PPD after intragastric (50 mg kg −1 ) and intravenous (4 mg kg −1 ) administration in rats. PPD showed rapid excretion and with bioavailability of simply about 5.7% in rats.
研究领域:
分析化学
·
药理学
·
中药学
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DOI
PubMed
高影响因子
MOLECULES
·
2022
·Vol. 27
·期 19
·6530
·
IF 4.927
Rui Li,Yanqing Zhang,Yanhong Li,Zihao Chen,Zhen Wang,Minghua Wang
As a chiral piperidine fungicide, fenpropidin has been widely used to control plant diseases. However, there are rare studies that have investigated fenpropidin at the enantiomer level. In this study, the single-factor analysis combined with a Box-Behnken design was used to obtain the optimal enantio-separation parameters of the fenpropidin enantiomers on ultra-performance liquid chromatography-tandem mass spectrometry. The absolute configuration of two fenpropidin enantiomers was confirmed for the first time using electron circular dichroism and optical activity. On the Lux cellulose-3 column,S-(-)-fenpropidin flowed out beforeR-(+)-fenpropidin. The enantio-separation mechanism was revealed by molecular docking. A modified QuEChERS method was developed for the trace determination of the fenpropidin enantiomers in seven food and environmental substrates. The average recoveries were 71.5–106.1% with the intra-day and inter-day relative standard deviations of 0.3–8.9% and 0.5–8.0%. The method was successfully verified by enantioselective dissipation of fenpropidin in soil under the field.R-(+)-fenpropidin dissipated faster thanS-(-)-fenpropidin, and the half-lives were 19.8 d and 22.4 d. This study established a brand-new effective chiral analysis method for the fenpropidin enantiomers, providing a basis for accurate residue monitoring and the risk assessment of fenpropidin.Keywords:fenpropidin;enantio-separation;absolute configuration;Box-Behnken design;enantioselective dissipation;molecular docking
研究领域:
分析化学
·
环境科学
·
农药学
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DOI
PubMed
高影响因子
Journal of Immunology Research
·
2020
·
IF 3.327
Yanan Shi,Jingming Xu,Bin Ding,Guiping Chen,Lu Jin,Liang Ke,Xiao Xu,JingXia Wang,Qiuhua Sun,Xiaohong Xu
Constipation, a gastrointestinal function disorder, is one of the side effects of paclitaxel (PTX) chemotherapy. Shenhuang plaster (SHP) application on the Shenque acupoint promotes gut motility in clinical settings. In this study, we elucidated the ingredients in SHP and evaluated its effects on PTX-induced constipation using a tumour-bearing mouse model. SHP was prepared using the traditional Chinese plaster preparation method. The ingredients were analysed using UPLC-MS/MS and identified via screening in a standard drug database. The gastrointestinal transit was evaluated by the movement of a fluorescein-labelled dextran in the gastrointestinal tract. A histological study of the mucosa was carried out after haematoxylin and eosin staining. mRNA expression was assessed using real-time RT-PCR, and the foetal microbiota composition was elucidated through 16 s rDNA sequencing and BLAST analysis. Our results indicate that the application of SHP attenuated weight gain inhibition by PTX; however, no inhibitory effect was observed on tumour growth. PTX-induced sluggish intestine, villus, and mucosal base layer damage were significantly improved following the application of SHP. Further, SHP enhanced the stimulation efficiency of PTX on TLR4 and its downstream cytokines, as well as on IL-1β in intestinal cells. SHP combined with PTX reshaped the microbiota, which showed beneficial effects on health. Hence, these results provide evidence that SHP alleviates PTX-induced constipation and intestinal morphological damage but augments the effects of PTX on the expression of cytokines in the TLR4 pathway and IL-1β. Therefore, we propose that SHP stimulates the host immune response to eradicate cancer cells.
研究领域:
药理学
·
肿瘤学
·
中医
·
胃肠病学
·
免疫学
·
微生物学
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Hao Zhou,Jiahao Li,Qi Shan,Cheng Zhao,Feng Xu,Qing Wang,Jiawei Lin,Yi Yin
Acylanilide fungicides are widely used in agricultural and aquaculture, so the determination of their residues is crucial for ensuring the quality and safety of agricultural products. In this work, a molecularly imprinted polymer (MIP) for the selective extraction of acylanilide fungicides was synthesized using oxadixyl as a dummy template, with methacrylic acid and acrylamide as functional monomers. The synthesis conditions were optimized, and the resulting MIP exhibited excellent adsorption capacity (Q ≥ 50.3 mg·g −1 ) and high selectivity (IF > 5.5). The morphology and structure of the MIP were characterized, and its adsorption performance and mechanism were investigated. After optimizing the molecularly imprinted solid-phase extraction (MISPE) procedure, an MISPE-UPLC–MS/MS method was developed for the determination of benalaxyl, furalaxyl, metalaxyl and its metabolite metalaxyl acid in aquatic products. The method demonstrated good linearity ( r > 0.995), and limits of detection and quantification for the four analytes were 0.1–0.3 μg·kg −1 and 0.3–1.0 μg·kg −1 , respectively. Average recoveries of metalaxyl, metalaxyl acid, benalaxyl, and furalaxyl in six aquatic products (grass carp, snakehead, bullfrog, pond loach, dongfeng snail, and red swamp crayfish) were 95.2–103.4 %, 86.7–101.5 %, 94.6–103.7 %, and 92.7–106.9 %, respectively, with relative standard deviations below 11.2 %. This highly sensitive and selective method effectively eliminates matrix interferences from various complex samples, thereby offering a robust strategy for monitoring acylanilide fungicide residues.
研究领域:
分析化学
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环境科学
·
食品安全
·
农业化学
·
水产养殖
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DOI
高影响因子
Biomolecules
·
2025
·Vol. 15
·期 12
·1694
·
IF 4.8
Siyu Huang,Xiaorui Li,Xin Lu,Biao Kan
Polymyxins, including polymyxin B (PMB), are last-resort antibiotics against multidrug-resistant Gram-negative infections in humans and livestock. Residual polymyxins from wastewater and manure can accumulate in soil, facilitating the emergence and spread of polymyxin resistance.Paenibacillus polymyxa, a natural polymyxin producer used in crop cultivation, may increase soil polymyxin burden. Since PMB strongly adsorbs to soil, its reliable quantification has been challenging. To address this, the extraction solvent and solid-phase extraction procedure were optimized to improve recovery and reduce matrix effects. We developed and validated a UPLC-MS/MS method to quantify PMB in soil. The method showed linearity (10–1000 ng/g), with a limit of detection of 0.86 ng/g and a limit of quantification of 2.12 ng/g. Method validation confirmed acceptable analytical performance. A 28-day monitoring of PMB in soil inoculated with varyingP. polymyxadoses revealed a dose-dependent increase over the first 14 days, followed by a decline; PMB remained detectable on day 28. Ecological risk assessment using the risk quotient (RQ) indicated that PMB levels in the high-dose group (2 × 108CFU/100 g) approached the high-risk threshold (RQ ≥ 1) on day 14, while lower doses posed low to medium risk. This work provides a soil PMB quantification method and insight into the ecological risk ofP. polymyxaapplication.
研究领域:
环境科学
·
分析化学
·
微生物生态学
·
抗生素耐药性
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产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2026
·Vol. 31
·期 9
·1517
·
IF 5.1
Muhammad Junaid Rao,Kangjian Song,Sijiu He,Shirong He,Yuanqiao Li,Ima Mulyama Zainuddin,Yubo Chen,Xinnian Du,Wei Liu,Munsif Ali Shad,Maryam Tahira,Xiande Duan,Bingsong Zheng,Liuyuan Bao,Shunqiang Yang,Mingzheng Duan
Phenolic compounds are vital bioactive constituents in fruits, yet modern strawberry breeding has often reduced their diversity. Here, we employed a multi-omics approach integrating UPLC-MS/MS-based metabolomics and RNA-seq transcriptomics to investigate the divergence in phenolic profiles and their transcriptional regulation between a wild strawberry ( Fragaria nilgerrensis , HM) and three cultivated varieties (white ‘Danxue’ (DX), pink ‘Fenyu’ (FY), and red ‘Red Face 99’ (RF)). The wild HM genotype exhibited higher antioxidant activity and a significantly more complex phenolic profile, dominated by high-abundance galloylated and benzoylated glucosides (e.g., digallic acid methyl ester, salicylic acid-2- O -glucoside) that were largely absent or depleted in cultivated fruits. In contrast, the cultivated varieties displayed specialized yet simplified profiles: DX accumulated hydroxycinnamoyl galactonic acids, FY was enriched in feruloylated glucosides, and RF was characterized by coumaroyl-glucose derivatives. Transcriptomic analysis identified a set of MYB transcription factors (e.g., FxaYL_531g0581170 , FxaYL_642g0175720 ) significantly upregulated in wild HM, with strong correlations to key bioactive phenolics such as 4-hydroxybenzoate and salicylic acid derivatives. These findings illustrate how selective breeding has reshaped phenolic composition through alterations in MYB regulatory networks. The wild strawberry germplasm thus represents a valuable natural reservoir for biofortification strategies aimed at restoring the nutritional and functional quality of modern strawberry cultivars.
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PubMed
高影响因子
危险品化学品经营许可证（带存储）