JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Yue Xiao,Shuai Yuan,Ruxin Luo,Ruiqin Zhu,Qiongying Zheng,Bin Di,Ping Xiang
The rapid global spread of new psychoactive substances (NPS) in recent years has become an issue in many countries. One emerging technology that can provide early warnings and assessments of drug situations is the monitoring of NPS in wastewater. In this study, we developed and optimized a high-throughput qualitative screening method based on direct injection that enabled the simultaneous detection of 311 NPS and metabolites (87 synthetic cannabinoids, 43 synthetic cathinones, 71 phenylethylamines, 10 tryptamines, 40 phencyclidines, 9 benzodiazepines, 38 fentanyls, and 13 piperazines) in municipal wastewater. The run time for drug detection was only 16 min, and the method was validated to perform well in terms of selectivity, limit of detection (LOD), recovery, and matrix effect. Overall, 95.8 % of the targets had an LOD ≤10 ng/L and the recoveries ranged from 71.01 % to 119.88 %. The method was validated on 976 real samples from a city in China, and 32 substances were detected, with the highest detection rate for ketamine. This study provides a simple and direct analytical method for wastewater monitoring, which will aid in combating drug-related crime and maintaining social stability as new NPS continue to enter global markets.
研究领域:
环境科学
·
毒理学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
International Journal of Analytical Chemistry
·
2020
·
IF 1.678
Zhenzhen Ying,Jingyao Wei,Ruijuan Liu,Fang Zhao,Yifang Yu,Xin Tian
Osimertinib is a novel oral, potent, and irreversible epidermal growth factor receptor tyrosine kinase inhibitor (EGFR-TKI) for treatment of advanced T790M mutation-positive advanced non-small cell lung cancer, which is commonly combined with ginsenoside Rg3 in clinic to enhance the efficacy and minimize adverse reactions. In the present study, a highly sensitive UPLC-MS/MS method was established and validated for analysis of osimertinib in rat plasma according to US FDA guideline. Separation was performed on a C18 (2.1 × 50 mm, 2.6 μm) column using a gradient elution of ammonium formate (10 mM) with 0.1% formic acid buffer (A) and ACN (B) at a flow rate of 0.2 mL/min. Detection was carried out on a triple quadrupole tandem mass spectrometer equipped with electrospray ionization in the MRM mode. The method was validated over a concentration range of 1–400 ng/mL for osimertinib. The intra- and interday accuracy and precision values were within ±15%. No significant degradation occurred under the experimental conditions in stability assays. There was a further investigation on the effects of multiple doses of ginsenoside Rg3 on the pharmacokinetics of osimertinib in rats for the first time. The results implied that osimertinib exhibited a slow absorption and moderate-rate elimination in rats following oral administration. Coadministeration with ginsenoside Rg3 (5 mg/kg, 7 days, i.g.) may have no effect on the pharmacokinetics of osimertinib in rats. The results provide a reference for the clinical concomitant medications of Rg3 and osimertinib.
研究领域:
药物分析
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肿瘤学
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药理学
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产品关联
DOI
PubMed
高影响因子
Food Bioscience
·
2024
·
IF 4.8
Baocheng Ji,Lanrui Yang,Mengxian Zhang,Peiyu Li,Zhuchen Hou,Jia Lv,Xu Xu,Wenbao Bi,Gaigai Xu,Yanhong Bai
In this study, a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method based on two kinds of silanized melamine sponges coupled with ultra-high liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) were developed for the determination of multiple pesticides and veterinary drugs in honey. Quick and convenient matrix separation could be achieved with the developed silanized melamine sponges by simply soaking and squeezing. At three spiked levels, all recoveries of the monitored drugs ranged from 63.6% to 114.8%, with relative standard deviations less than 17.7%. No significant matrix influence was observed with matrix effects within −13.9%∼+15.1% for all monitored drugs. Good linearity with correlation coefficient (R 2 ) ≥0.991 was obtained in the range of 0.08–100 μg kg −1 for most drugs. The limits of detection and quantification ranged from 0.04 to 3.6 μg⋅kg −1 and from 0.08 to 9.8 μg⋅kg −1 , respectively. The results had shown the satisfactory matrix purification performance of silanized melamine sponges and indicated its good application prospect in the multiple determination of pesticides and veterinary drugs in various foods.
研究领域:
食品科学
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分析化学
✓ 已验证
产品关联
DOI
高影响因子
CyTA-Journal of Food
·
2022
·
IF 2.478
Yanzhi Sun,Yingjie Fu,Rirong Chen,Yipeng Zhang,Tougen Liao,Hui Xi,Shihao Sun,Zhihong Cheng
The systematic identification of volatile organic compounds (VOCs) and non-VOCs will facilitate understanding the characteristic aroma and bioactive constituents of Dianhong. This article reported for the first time the volatile and non-volatile composition profiles of Dianhong from four main producing areas. A combined total of 42 VOCs were identified from four Dianhong samples by static headspace GC-MS. Thirteen VOCs were found to be important common components contributing to the characteristic aroma of Dianhong. The non-VOCs of Dianhong were evaluated by UPLC-ESI-MS, and Dianhong samples from four producing areas shared almost the same component profiles. Thirty-four components including derivatives of quinic acid, gallic acid, and catechin, flavone C-glycosides, flavonol O-glycosides, and alkaloids were characterized. Finally, catechin, gallic acid, 5-O-galloylquininc acid, and theobromine were characterized as the main non-VOCs in Dianhong. Dianhong samples from four main producing areas showed similar VOCs and non-VOCs profiles under our optimized GC-MS and LC-MS conditions.
研究领域:
食品科学
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分析化学
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植物学
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Ting Tao,Yuyu Cao,Liping Zhang,Dayi Xu,Kaiyuan Pang,Yanli Li,Xiaobao Wei,Zengxian Sun
Thiol amino acids, with great physiological significance, are unstable, and have small molecular weights, as well as very low endogenous concentrations. Therefore, to quantitatively and directly analyze them using liquid chromatography-tandem mass spectrometry is difficult. To overcome these problems, we aimed to prepare a thiol-free amino acid plasm matrix as blank sample to reduce the background for the first time. Using compounds with maleimide group that react with classical thiols to generate water-insoluble products. Reducing agents Tris(2-carboxyethyl)phosphine (TCEP) was applied to cooperate with bismaleimide (DM) for elimination of thiol amino acids from plasma 10 min at room temperature and pH 7. Further, the residual TCEP from plasma were removed using an anion exchange resin within 10 min. Methodological validation analysis revealed good performance in linearity, precision, extraction recovery (≥ 82 %), and stability (except oxidized glutathione). This quantitative analysis was successfully applied to blood samples of 9 people in good health. This study provides a foundation for the development of accurate and rigorous quantitative analysis methods targeting thiol amino acids in different body fluids or tissues. Moreover, it paves the way toward realizing several clinical applications.
研究领域:
生物化学
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临床医学
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产品关联
DOI
PubMed
高影响因子
Frontiers in Pharmacology
·
2025
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IF 4.8
Fengyichi Zhang,Fanxi Guo,Xinyu Zhao,Chongyang Li,Junli Wang,Mengyun Wang,Ruixia Ma,Baochang Chen,Qiangqiang Miao,Yimeng Wang,Zihan Wang,Di Cao,Zugong Yu
A rapid, sensitive and reliable ultra–performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) was developed and validated for the simultaneous quantitation of pyrantel (PYR), praziquantel (PRA), febantel (FBT) and its active metabolites, fenbendazole (FEN) and oxfendazole (OXF) in dog plasma. Fenbendazole–D3 (FEN–D3) was used as an internal standard (IS). The analytes and IS were prepared using simple protein precipitation (PP) combined with liquid–liquid extraction (LLE). Chromatographic analysis was performed on UPLC BEH C18 column using acetonitrile–0.1% formic acid in water for gradient elution. Detection was carried out in multiple reaction monitoring (MRM) mode under positive electrospray ionization. The standard curves were linear through the concentration range of 4–240 ng/mL for PYR and OXF, 15–900 ng/mL for PRA, 2–120 ng/mL for FBT and 10–600 ng/mL for FEN with all correlation coefficients >0.99. The intra–and inter–batch precision was 1.08%–14.26% and accuracy was from 90.66% to 110.28%. The mean extraction recoveries for the analytes and IS were >90%. The total run time was 9.0 min. The developed method was successfully applied to a bioequivalence study after oral administration of compound febantel tablets in 38 healthy dogs.
研究领域:
兽医学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2025
·
IF 3.1
Sai Li,Shuangying Yu,Mengyao Zhang,Zeyi Li,Hui Yu,Zhongfu Xing,Beibei Mao,Pan Zhao
In this study, biochars with desirable adsorption capacity were prepared by calcination of herbal medicine residue, and the obtained biochars were loaded on cellulose aerogel through a green synthesis method. The monolithic biochar/cellulose aerogel hybrid was packed in the syringe and used as adsorbent for microextraction in packed syringe (MEPS). After introducing cellulose aerogel as the support, the loss of powdered biochars was avoided, and the entire extraction process can be achieved through simple operation of filtration due to the macroporous structure of cellulose aerogel. Coupled with UPLC-MS/MS, the established method was successfully applied to determine trace level of sulfonamides (SAs) in water samples. Extraction parameters such as pH of sample solution, adsorbent type, sample volume, elution solvent type and elution solvent volume were studied. Under the optimized parameters (pH of sample solution:7, adsorbent type: biochar/cellulose aerogel, sample volume: 20 mL, elution solvent: 0.3 mL methanol, the number of aspiration and dispense of sample solution, washing solvent and elution solvent: 3), desirable linearity correlation coefficient (r) in the range of 0.9951–0.9972 was achieved. The limit of detection varied from 0.00407 to 0.0104 ng/mL, and recovery ranging from 65.3 % to 102.4 % was obtained. The proposed method was demonstrated to be sensitive, accurate and easily operative, providing a convenient protocol for sample pretreatment.
研究领域:
环境科学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2022
·Vol. 27
·期 19
·6190
·
IF 4.927
Xueru He,Ying Li,Yinling Ma,Yuhao Fu,Xuejiao Xun,Yanjun Cui,Zhanjun Dong
Sorafenib (SOR), an inhibitor of multiple kinases, is a classic targeted drug for advanced hepatocellular carcinoma (HCC) which often coexists with type 2 diabetes mellitus (T2DM). Dapagliflozin (DAPA), a sodium–glucose cotransporter-2 inhibitor (SGLT2i), is widely used in patients with T2DM. Notably, co-administration of SOR with DAPA is common in clinical settings. Uridine diphosphate-glucuronosyltransferase family 1 member A9 (UGT1A9) is involved in the metabolism of SOR and dapagliflozin (DAPA), and SOR is the inhibitor of UGT1A1 and UGT1A9 (in vitro). Therefore, changes in UGT1A9 activity caused by SOR may lead to pharmacokinetic interactions between the two drugs. The objective of the current study was to develop an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of SOR and DAPA in plasma and to evaluate the effect of the co-administration of SOR and DAPA on their individual pharmacokinetic properties and the mechanism involved. The rats were divided into four groups: SOR (100 mg/kg) alone and co-administered with DAPA (1 mg/kg) for seven days, and DAPA (1 mg/kg) alone and co-administered with SOR (100 mg/kg) for seven days. Liquid–liquid extraction (LLE) was performed for plasma sample preparation, and the chromatographic separation was conducted on Waters XSelect HSS T3 column with a gradient elution of 0.1% formic acid and 5 mM ammonium acetate (Phase A) and acetonitrile (Phase B). The levels of Ugt1a7 messenger RNA (mRNA) were determined in rat liver and intestine using quantitative real-time polymerase chain reaction (qRT-PCR). The method was successfully applied to the study of pharmacokinetic interactions. DAPA caused a significant decrease in the maximum plasma concentrations (Cmax) and the area under the plasma concentration–time curves (AUC0–t) of SOR by 41.6% and 50.5%, respectively, while the apparent volume of distribution (Vz/F) and apparent clearance (CLz/F) significantly increased 2.85- and 1.98-fold, respectively. When co-administering DAPA with SOR, the AUC0–tand the elimination half-life (t1/2Z) of DAPA significantly increased 1.66- and 1.80-fold, respectively, whereas the CLz/Fsignificantly decreased by 40%. Results from qRT-PCR showed that, compared with control, seven days of SOR pretreatment decreased Ugt1a7 expression in both liver and intestine tissue. In contrast, seven days of DAPA pretreatment decreased Ugt1a7 expression only in liver tissue. Therefore, pharmacokinetic interactions exist between long-term use of SOR with DAPA, and UGT1A9 may be the targets mediating the interaction. Active surveillance for the treatment outcomes and adverse reactions are required.Keywords:UPLC-MS/MS;sorafenib;dapagliflozin;pharmacokinetics;drug–drug interactions
研究领域:
药理学
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临床药学
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分子生物学
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药物代谢
✓ 已验证
产品关联
DOI
PubMed
高影响因子
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
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分析化学
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营养学
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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
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代谢
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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
危险品化学品经营许可证（带存储）