Frontiers in Chemistry
·
2021
·
IF 5.221
Chang Xiangwei,Zhang Zhenyu,Yan Hui,Su Shulan,Wei Dandan,Guo Sheng,Shang Erxin,Sun Xiaodong,Gui Shuangying,Duan Jinao
Nucleobases, nucleosides, nucleotides and amino acids, as crucial nutrient compositions, play essential roles in determining the flavor, function and quality of Chrysanthemi Flos. The quality of Chrysanthemi Flos from different geographical origins is uneven, but there have been no reports about the screening of their quality markers based on nutritional ingredients. Here, we developed a comprehensive strategy integrating ultra performance liquid chromatography coupled with triple-quadrupole linear ion-trap tandem mass spectrometry (UPLC–MS/MS) and multivariate statistical analysis to explore quality markers of Chrysanthemi Flos from different geographical origins and conduct quality evaluation and discrimination of them. Firstly, a fast, sensitive, and reliable UPLC–MS/MS method was established for simultaneous quantification 28 nucleobases, nucleosides, nucleotides and amino acids of Chrysanthemi Flos from nine different regions in China. The results demonstrated that Chrysanthemi Flos from nine different cultivation regions were rich in the above 28 nutritional contents and their contents were obvious different; however, correlation analysis showed that altitude was not the main factor for these differences, which required further investigation. Subsequently, eight crucial quality markers for nine different geographical origins of Chrysanthemi Flos, namely, 2′-deoxyadenosine, guanosine, adenosine 3′,5′-cyclic phosphate (cAMP), guanosine 3′,5′-cyclic monophosphate (cGMP), arginine, proline, glutamate and tryptophan, were screened for the first time using partial least squares discriminant analysis (PLS-DA) and the plot of variable importance for projection (VIP). Moreover, a hierarchical clustering analysis heat map was employed to intuitively clarify the distribution of eight quality markers in the nine different regions of Chrysanthemi Flos. Finally, based on the contents of selected eight quality markers, support vector machines (SVM) model was established to predict the geographical origins of Chrysanthemi Flos, which yielded excellent prediction performance with an average prediction accuracy of 100%. Taken together, the proposed strategy was suitable to discover the quality markers of Chrysanthemi Flos and could be used to discriminate its geographical origin.
研究领域:
中药学
·
分析化学
·
营养学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF FOOD SCIENCE AND TECHNOLOGY
·
2020
·Vol. 56
·期 6
·2983-2991
·
IF 2.773
Shujie Wang,Guoqin Liu,Weiwei Cheng
Summary This research investigated the effect of carnosic acid (CA), tert-butyl hydroquinone (TBHQ), sesamol (SL) and L-ascorbyl palmitate (AP) on the inhibition of glycidyl esters (GEs) and oxidation parameter changes in rice bran oil (RBO) during heat processing. The electron spin resonance (ESR) analysis showed that the free radical scavenging ability of them was ranked as CA > TBHQ > SL > AP. With the addition of CA, TBHQ, SL and AP (0.6 g kg −1 ), the GEs content was reduced significantly from 987.98 ± 8.45 to 283.87 ± 4.78, 303.21 ± 4.38, 440.52 ± 3.82 and 500.55 ± 2.99 μg kg −1 , respectively. All four free radical scavengers had the highest inhibitory effect on C18:2-GE, followed by C18:1-GE and C16:0-GE. Moreover, the free radical scavengers were also effective to inhibit oil oxidation. Overall, the natural-free radical scavenger may be a promising candidate to mitigate GE formation and oil oxidation due to its effectiveness and safety.
研究领域:
食品科学
·
化学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Yingxia Guo,Jiaxin Zhang,Runran Mei,Zihan Tang,Meichen Liu,Xixian Weng,Meiyun Shi,Lei Yin
Addressing critical gaps in understanding the in vivo behavior of polyethylene glycol (PEG)-based excipients, this study systematically elucidates the biological fate of methoxy-PEG₆-hydroxyl (M-PEG₆-OH) through comprehensive pharmacokinetic and metabolic investigations in rats. Employing a validated ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) methodology, we reveal distinctive biodistribution characteristics including rapid systemic clearance (Half-life (t 1/2 ) = 1.92 ± 1.16 h) and extensive tissue penetration (Apparent volume of distribution (V d ) = 0.84 ± 0.45 L/kg), suggesting efficient extravascular dissemination. Excretion pathways analysis demonstrated predominant renal elimination, with 59.03 % of the administered dose recovered in urine within 48 h post-IV injection, contrasting with minimal fecal excretion (0.99 %). Quantitative metabolite profiling identified M-PEG₅-CH₂COOH as the oxidative transformation product through terminal hydroxyl modification. The significantly higher relative abundance of metabolites (M-PEG 5 -CH 2 COOH) in urine compared to feces within the same time period provides critical insights into the biotransformation processes and metabolic pathways of the PEG polymer. These findings establish the first systematic evidence of metabolic trajectory and elimination mechanisms for M-PEG-OH, offering vital references for optimizing PEGylated drug delivery systems with enhanced biocompatibility and predictable safety profiles.
研究领域:
药代动力学
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分析化学
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生物化学
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药剂学
·
代谢
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2016
·Vol. 8
·期 17
·3550-3563
·
IF 1.915
Man-Yun Chen,Yong-Jun Tang,Yi-Cheng Wang,Chong-Zhi Wang,Chun-Su Yuan,Yao Chen,Zhi-Rong Tan,Wei-Hua Huang,Hong-Hao Zhou
The compound medicine of betamethasone sodium phosphate (BSP) and betamethasone dipropionate (BDP) is widely used for the treatment of diverse glucocorticoid-sensitive acute and chronic diseases such as asthma, rheumatoid arthritis and systemic lupus erythematosus. It will be useful and beneficial to validate a sensitive method for the determination of BSP, BDP and their metabolites for a pharmacokinetic study. Hereby, ultra-high pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been validated for the determination of BSP, BDP and their metabolites betamethasone (BOH), betamethasone 17-monodipropionate (B17P) and betamethasone 21-monodipropionate (B21P) in human plasma. Liquid–liquid extraction with ether and n-hexane (v/v, 4 : 1) was used for sample preparation of BDP, BOH, B17P and B21P with beclomethasone dipropionate as the internal standard (IS), while solid phase extraction was adopted for sample preparation of BSP using prednisolone as the IS. Chromatographic separation was performed on a Hypurity C18 column (150 mm × 2.1 mm, 5 μm) for BOH, BDP, B21P and B17P, and a Luna C18 (2) column (150 mm × 2.0 mm, 5 μm) for BSP. Electrospray ionization interfaced with positive multiple reaction monitoring (MRM) scan mode was used for mass spectrometric detection. The standard calibration curves were linear within the range of 2.525 × 10−9 to 403.9 × 10−9 mol dm−3 for BSP, 0.125 × 10−9 to 55.81 × 10−9 mol dm−3 for BDP, 0.278 × 10−9 to 74.95 × 10−9 mol dm−3 for BOH, 0.098 × 10−9 to 4.688 × 10−9 mol dm−3 for B17P and 0.226 × 10−9 to 5.411 × 10−9 mol dm−3 for B21P, respectively. The validated method was successfully applied to a bioequivalence study in 23 healthy subjects after they were injected with this compound medicine BSP and BDP.
研究领域:
药物分析
·
临床药理学
✓ 已验证
DOI
PubMed
高影响因子
Current Pharmaceutical Analysis
·
2023
·Vol. 19
·期 6
·511-520
·
IF 0.6
Zhang Mengmeng,Zou Qiaogen
Background: Atopic dermatitis (AD) is an allergic skin disease that can be inherited. Crisaborole is a specific drug developed to deal with this disease. The compounds of 4-(4- Bromo-3-formyl-phenoxy)-benzonitrile and 4-(4-(4-bromo-3-formylphenoxy)-3- formylphenoxy) benzonitrile
are the representative impurities in the synthesis of Crisaborole active pharmaceutical in gradient (API). Owing to the genotoxic impurities that could lead to cancer and gene mutations, it is necessary to develop a simple, efficient, sensitive, and accurate method to detect these impurities.
In this study, the 4-(4-Bromo-3-formyl-phenoxy)-benzonitrile and 4-(4-(4- bromo-3-formylphenoxy)-3-formylphenoxy)benzo- nitrile present in Crisaborole API were detected using UPLC-MS/MS. Methods: The separation was made on a ZORBAX Eclipse XDB-Pheny column (4.6 mm ×75mm, 3.5
μm) with the mobile phase of acetonitrile solution containing 0.1% trifluoroacetic acid (A) and water containing 0.1% formic acid (B) in gradient elution mode. Quantification was performed using positive ion electrospray ionization (ESI), and the contents of two compounds were determined
using the multiple reaction monitoring (MRM) modes. Results: The quantitative analytical method was fully validated with respect to linearity (r > 0.9998), sensitivity, precision, accuracy (the average recovery of two impurities was 84.1% to 90.7%), and robustness. Conclusion:
Three batches of samples were detected by UPLC-MS/MS, indicating that the proposed approach was applicable for the quality evaluation of Crisaborole.
研究领域:
药物分析
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皮肤病学
·
毒理学
✓ 已验证
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Yan Qiao,Menglin Wang,Erling Guo,Ke Wang,Ling Ma,Kaoqi Lian
This study aimed to design and synthesize a novel adsorbent Fe 3 O 4 @SiO 2 @MPA-TAPA-COF material for the first time and used as an adsorbent of MSPE. It had significant potential for the pretreatment of trace analytes. The MSPE was coupled with ultra performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) for the rapid extraction and detection of 12 sulfonamides (SAs) from water and milk samples for the first time. Several experimental parameters were optimized, including adsorbent dosage and the effects of pH, ionic strength, adsorption time, and desorption conditions. Under the optimized pretreatment and instrumental conditions, good linearity of 0.1–100 μg·L −1 with a correlation coefficient 0.9994–0.9999, low limits of detection (0.004–0.044 μg·L −1 ) and limits of quantitation (0.013–0.136 μg·L −1 ) were obtained. Moreover, the recoveries of sulfonamides in water and milk samples were in the range of 60.88 %-102.94 %, and the relative standard deviations not exceeding 9.62 %. Finally, the magnetic Fe 3 O 4 @SiO 2 @MPA-TAPA-COF material possessed the magnetic separation and high adsorption affinity for extracting SAs from real samples. This study holds great significance in enhancing the monitoring of SAs drug residues in water and milk.
研究领域:
分析化学
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环境科学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Xiaoxue Liu,Chenrong Huang,Ling Xue,Qingqing Xu,Wen Xia,Xing Li,Liyan Miao
A rapid and highly sensitive liquid chromatography-tandem mass spectrometry (LC–MS/MS) method has been developed and validated for the determination of a novel anti-HBV compound Y101 and its metabolites M8 and M9 in human plasma. The plasma samples were deproteinated with acetonitrile after addition of Peramivir (internal standard, IS) and separated on a 40 °C ACQUITY UPLC BEH C 18 column (2.1 mm × 50 mm, 1.7 μm). The mobile phase consisted of water (containing 5 mM ammonium acetate and 0.1% formic acid) and acetonitrile (74:26, v/v) at a flow rate of 0.3 mL/min. The detection was performed on a Triple Quad 5500 tandem mass spectrometer coupled with electrospray ionization (ESI) source in positive mode. Quantification was conducted by multiple reaction monitoring (MRM) of the transitions of m / z 490.1 → 339.0 for Y101, m / z 357.2 → 105.2 for metabolite M8, m / z 373.1 → 105.1 for metabolite M9 and m / z 329.1 → 270.2 for IS, respectively. The method was validated over the calibration curve range of 1.000–1000 ng/mL for Y101, 2.000–2000 ng/mL for metabolite M8 and 0.3000–300.0 ng/mL for metabolite M9, using linear regression and 1/x 2 weighting. No matrix effect and carryover effect was observed. The intra- and inter-batch precision and accuracy of Y101, metabolite M8 and M9 were all within the acceptable criteria. This method allows a rapid and simple determination of Y101 and its metabolites M8 and M9 in human plasma. It was successfully applied in a pharmacokinetic study in human for the first time.
研究领域:
药理学
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分析化学
·
临床药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Weihao Ma,Hao Zhang,Jiayuan Nie,Chunyu Qiang,Zhiwei Li,Ling Ma,Ke Wang
In this study, a novel magnetic covalent organic framework (Fe 3 O 4 @SiO 2 -HBTA-TTA-COF) was synthesized, which was fully characterized by scanning electron microscopy, transmission electron microscopy, etc. Furthermore, a new method was developed for the determination of 25 quinolones (QNs) in water and milk using the Fe 3 O 4 @SiO 2 -HBTA-TTA-COF as magnetic solid-phase extraction adsorbent coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Meanwhile, various experimental parameters were optimized including sample solution pH, adsorbent dosage and extraction time, etc. Under the optimal conditions, good linearity in the range of 0.1–200 μg·L −1 (R 2 ≥ 0.999) were obtained, the recoveries of 25 QNs were 70.04 %–104.4 % with the relative standard deviations lower than 9.87 % (n = 5), the limits of detection were 0.003–0.010 μg·L −1 for water and 0.018–0.722 μg·kg −1 for milk. This established method was high-sensitive and high-throughput, which can be used as a good alternative method for the selective determination of 25 QNs in water and milk.
研究领域:
分析化学
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环境科学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2015
·
IF 2.979
Min Liao,Cong Dai,Mengping Liu,Jiefeng Chen,Zuanguang Chen,Zhiyong Xie,Meicun Yao
A novel, sensitive and rapid ultra-performance liquid chromatography–tandem mass spectrometric (UPLC–MS/MS) method for simultaneous quantification of four furostanol glycosides in rat plasma was established and validated. Ginsenoside Rb1 was used as an internal standard. Plasma samples were pretreated by liquid–liquid extraction with n -butanol and chromatographed on a C18 column (2.1 × 50 mm i.d., 2.6 μm) using a gradient elution program consisting of acetonitrile and water (containing 0.03% formic acid and 0.1 mM lithium acetate) at a flow rate of 0.4 mL/min. Lithium adduct ions were employed to enhance the response of the analytes in electrospray positive ionization mode and multiple reaction monitoring transitions were performed for detection. All calibration curves exhibited good linearity ( r > 0.999) over the range of 10–20,000 ng/mL for protodioscin and 2–4000 ng/mL for protogracillin, pseudoprotodioscin and pseudoprotogracillin. The recoveries of the whole analytes were more than 80.3% and exhibited no severe matrix effect. Meanwhile, the intra- and inter-day precisions were all less than 10.7% and accuracies were within the range of −8.1–12.9%. The four saponins showed rapid excretion and relative high plasma concentrations when the validated method was applied to the PK study of Dioscorea nipponica extracts by intragastric administration at low, medium and high dose to rats. Moreover, the T 1/2 and AUC 0– t of each compound turned out to behave in a dose-dependent pattern by comparing them at different dose levels.
研究领域:
分析化学
·
药理学
✓ 已验证
DOI
PubMed
高影响因子
TALANTA
·
2016
·
IF 4.035
Xinpeng Dai,Xiuna Jia,Pan Zhao,Ting Wang,Jian Wang,Peiting Huang,Lu He,Xiaohong Hou
As a novel kind of materials, metal-organic frameworks (MOFs) have great potential for the preconcentration of trace analytes. In our work, MIL-101(Cr) was prepared and applied as a solid phase extraction (SPE) sorbent for the pretreatment of sulfadiazine (SDA), sulfamethazine (SMZ), sulfachloropyridazine (SCP) and sulfamethoxazole (SMX) in different environmental water samples coupling with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) detection. Experimental parameters, such as SPE materials, pH of water sample, volume of sample, flow rate , and type and volume of elution solvent, were properly optimized. Under the optimum conditions, good sensitivity levels were achieved with the detection limits of 0.03–0.08 μg/L and the quantitation limits of 0.11–0.27 μg/L. The linear ranges were from 0.2–40 or 0.5–100 μg/L ( r 2 >0.996) for the analytes, and the relative recoveries were in the range from 83.5% to 107.3% with the relative standard deviations (RSD) between 0.2% and 8.0% ( n =6). In addition, computational simulation was primarily used to predict the adsorption of MIL-101(Cr) toward sulphonamides (SAs), and also demonstrated the molecular interactions and free binding energies with the molecular modeling method. The results revealed that the combination of experimental and computational study not only accurately recognized the adsorption of MIL-101(Cr) on SAs, but also provided a new strategy on the trace contaminant analysis.
研究领域:
环境科学
·
分析化学
✓ 已验证
DOI
高影响因子
Analytical Methods
·
2025
·
IF 2.6
Jieting Zhang,Shuo Diao,Zhen Huang,Mengyuan Wu,Xintong Wang,Yiran Zhao,Mingming Yu,Xianzhen Wang,Jingchun Yao,Guimin Zhang,Sherwin K. B. Sy,Zhihua Lv,Hai Yang
Guided by the principles of Analytical Quality by Design (AQbD), a highly selective and sensitive LC-MS/MS method was established for the simultaneous quantification of 15 compounds in Shouhui Tongbian capsules, enabling their effective quality control. The separation was carried out on a BEH C18 column (1.7 μm, 2.1 × 100 mm) with a mobile phase comprising 0.1% formic acid in 3 mM ammonium acetate aqueous solution and methanol (60 : 40, v/v) at a flow rate of 0.30 mL min−1. The method exhibited good linearity within a certain concentration range (R2 > 0.9906) depending on the compound; the precision ranged from 0.6% to 14.7% and accuracy was within 11.2%. Among the 15 detected compounds, aloin had the highest content in the Shouhui Tongbian capsules, reaching 227.3780 mg g−1, followed by betaine and L-hydroxyproline, with concentrations of 1.3204 mg g−1 and 1.2929 mg g−1, respectively. This method simultaneously detected the content of 15 compounds in five batches of Shouhui Tongbian capsules.
研究领域:
分析化学
·
药物分析
·
质量控制
·
色谱-质谱分析
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中医药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2021
·
IF 3.935
Menghua Zhang,Xiaoxue Liu,Zhiyao Chen,Shenhao Jiang,Lin Wang,Min Tao,Liyan Miao
Over the past decades, therapeutic drug monitoring (TDM) of tyrosine kinase inhibitors (TKIs) and their main active metabolites has shown benefits in improving treatment efficacy and safety. Therefore, a sensitive, simple and economical ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the determination of six oral tyrosine kinase inhibitors (TKIs) and two active metabolites, including imatinib (IMA), N-desmethyl imatinib (NDIMA), sunitinib (SUNI), N-desethyl sunitinib (NDSUNI), regorafenib (REGO), nilotinib (NILO), dasatinib (DASA) and osimertinib (OSI) in human plasma/serum for therapeutic drug monitoring. The plasma/serum samples were deproteinated with acetonitrile after spiking with two deuterated internal standards (ISs, [ 2 H 8 ]-imatinib and [ 2 H 10 ]-sunitinib) and separated on a 40 °C ACQUITY UPLC® BEH C 18 column (1.7 µm, 2.1 mm × 50 mm). The mobile phase was composed of acetonitrile (solution A) and water-formic acid-ammonium acetate (1 M) (994:1:5, v/v/v, solution B). Gradient elution was applied at a flow rate of 0.4 mL/min. Detection was carried out using a Triple Quad 5500 tandem mass spectrometer coupled with an electrospray ionization (ESI) source in positive mode. The method was validated over the calibration curve (CV) range of 2–400 ng/mL for NDSUNI and DASA, 2.5–500 ng/mL for SUNI, 10–2000 ng/mL NDIMA and OSI, 20–4000 ng/mL for NILO, 30–6000 ng/mL for REGO and 50–10000 ng/mL for IMA using linear regression and 1/x 2 weighting. No difference was observed in the matrix effect (ME) among blank human plasma, hemolytic plasma, lipemic plasma, plasma spiked with ten commonly used drugs by cancer patients, or serum samples in general. The standard curve fitted by two standard curves of serum and plasma showed good linearity, and the precision and accuracy results of QC samples in both plasma and serum were acceptable and the concentration was comparable. To provide a clinical reference for the operation, the stability of the whole process from sample collection to drug detection was verified. SUNI and NDSUNI showed obvious photoisomerization under light exposure. Therefore, strict light protection was applied for all sample collection and handling steps of SUNI and NDSUNI. Compared with heparin anticoagulant tubes, the stability of the eight compounds in both whole blood and plasma was better in K3-EDTA and sodium citrate anticoagulant tubes. Given that all the analytes were stable in plasma at 4 °C for 48 h and in whole blood at room temperature for 48 h but OSI and REGO were unstable in whole blood and plasma at room temperature, samples should be centrifuged as soon as possible to be preserved as plasma at 4 °C when OSI or REGO is detected. In conclusion, this validated method can provide support for clinical practice, such as therapeutic drug monitoring (TDM) and pharmacokinetic studies of these six TKIs and two active metabolites.
研究领域:
药理学
·
临床医学
·
分析化学
✓ 已验证
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）