Heliyon
·
2024
·
IF 3.4
Shunqin Chen,Han Yang,Shan Zhang,Faze Zhu,Shan Liu,Huan Gao,Qing Diao,Wenbo Ding,Yuemeng Chen,Peng Luo,Yubo Liu
This study developed an online solid-phase extraction ultra-high performance liquid chromatography-tandem mass spectrometry (Online-SPE-UHPLC-MS/MS) method for the analysis of 28 illegal drugs in sewage. To achieve this, 28 isotope internal standards (ISTDs) were added to 3 mL sewage samples, the pH was adjusted to 7–8 using hydrochloric acid or 20% ammonia water, followed by centrifugation, filtration, and analysis using UHPLC-MS/MS. The results indicated an excellent linearity of 1–300 ng L −1 , and cotinine in the concentration range of 20–6000 ng L −1 , linear correlation coefficient R 2 > 0.995, with the limit of detection (LOD) of 0.01–6 ng L −1 , and a limit of quantification (LOQ) of 0.1–20 ng L −1 . The addition of three concentrates of low (2 ng L −1 /40 ng L −1 ), medium (20 ng L −1 /400 ng L −1 ), and high concentration (200 ng L −1 /4000 ng L −1 ) demonstrated the matrix effect of the target compound between ± 22.0%. The extraction recovery was 70.0–119.4%, and a percent accuracy of 75.7–118.1%. Similarly, the intra- and inter-day precisions were 1.8–20.0% and 1.5–18.9%, respectively. The results cemented the sensitivity, accuracy, reliability, strong specificity, and reproducibility, which can be used to screen 28 illegal drugs in sewage for trace analysis.
研究领域:
环境科学
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分析化学
·
毒理学
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PubMed
高影响因子
Journal of Natural Medicines
·
2026
·
IF 2.6
Mao Qiang,Zhong Huan,Liang Wan-Li,Dai Jin,Huang Rui-Ting,Wang Yi-Di,Sun Di-Yang,Tang Kai,Xia Long-Fei,Gong Hai-Biao,Li Yi-Fang,Sun Wan-Yang,Zhang Qiong-Yi,Zeng Li,Yu Li-Li,Xu You-Hua,Wu Qi-Biao,Zhu Yi-Zhun,Tan Hong-Li,Ouyang Shu-Hua,He Rong-Rong
Natural Calculus Bovis (NCB) and Bovis Calculus Sativus (BCS) are both used clinically but exhibit different therapeutic effects, the material basis of which remains unclear. Lipid-soluble components are hypothesized to contribute to these differences, however the compositional variations at the lipid level have not been fully characterized. In this study, untargeted UHPLC-MS/MS lipidomics was employed to compare the lipid profiles of NCB and BCS. The results indicated that both samples contained fatty acyls, glycerolipids (GL), glycerophospholipids (GP), sphingolipids (SP), and sterol lipids (ST), indicating a conserved core lipid framework. However, NCB showed higher lipid complexity and abundance. NCB contained higher levels and greater molecular diversity of intact GP (phosphatidylcholines and phosphatidylethanolamines), SP (ceramides), fatty acid-derived lipids (polyunsaturated N -acylethanolamines, PU-NAE), and sterol esters. In comparison, BCS exhibited a simplified profile dominated by GL, with reduced GP, SP and ST species, enrichment of lysophospholipids and bile acid-related sterols, and lower overall lipid abundance. These differences may result from distinct formation processes: prolonged in vivo maturation for NCB versus time-limited in vitro culturing for BCS. This study expands the current understanding of the material basis of NCB and BCS, from a lipidomic perspective, offering molecular insights into its pharmacological properties and providing a scientific foundation for the material basis, quality control, standardization and rational clinical application of Calculus Bovis . Graphical abstract The alternative text for this image may have been generated using AI.
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PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Yingxia Guo,Meichen Liu,Jiye Tian,Chunpeng Feng,Qingbin Wang,Xuan Zhao,Lei Yin
As an important chemical reagent, methoxy polyethylene glycol amine (mPEG-NH 2 ) is widely used in biomedical field. Unraveling the pharmacokinetic behavior of mPEG-NH 2 polymers is essential for revealing the toxicity and efficiency of mPEG-NH 2 related drug delivery systems. In this study, a simple analytical assay based on mass spectrometry (MS) was first established and validated for quantification of mPEG 5 -NH 2 in biological matrix. The multiple reaction monitoring (MRM) transitions at m / z 252.2 (precursor ions) → 87.7 (fragment ions) and m / z 371.2 (precursor ions) → 89.2 (fragment ions) were chosen to determine mPEG 5 -NH 2 and OH-PEG 8 -OH, respectively. The UHPLC-MS/MS assay showed excellent linearity over the range of 0.01–10 μg/mL. Intra-day and inter-day accuracies and precisions of the assay were all within ± 6.44 %. The analytical assay was successfully applied to reveal the in vivo pharmacokinetic behavior of mPEG 5 -NH 2 in rats.
研究领域:
药理学
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分析化学
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生物医学工程
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PubMed
高影响因子
DRUG METABOLISM AND DISPOSITION
·
2026
·
IF 4
Jiye Tian,Jiarui Zhang,Zihan Tang,Chunpeng Feng,Yue Deng,Jiale Liu,Shuang Feng,Xinyue Zhou,Lei Yin,Meiyun Shi
A comprehensive understanding of the in vivo fate of low-molecular-weight polyethylene glycol (PEG) oligomers is essential for optimizing PEGylated therapeutics. This study delineates the polymerization-dependent absorption, distribution, metabolism, and excretion (ADME) of discrete PEG600 oligomers (n = 9–18) in rats using a validated UHPLC-MS/MS method. Systemic exposure, assessed by dose-normalized AUC, was highest for shorter oligomers (n = 9–10) and declined for longer chains (n ≥ 17), while all oligomers exhibited similarly short terminal half-lives (12.7–15.2 min), indicating rapid elimination irrespective of chain length. Tissue distribution revealed pronounced renal accumulation, peaking at mid-chain lengths (n = 11–13), consistent with size-dependent glomerular filtration and tubular reabsorption. Oxidative metabolism yielded both mono- and di-carboxylated derivatives, confirming active enzymatic processing. Excretion studies demonstrated chain-length-dependent elimination, with reduced recovery of longer oligomers suggesting substantial in vivo biodegradation. These findings provide the first monomer-resolved ADME profile of PEG600 oligomers, highlighting the critical role of polymerization degree in governing their pharmacokinetics and informing the rational design of PEGylated drug formulations.
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2026
·
IF 3.1
Xiaoyan Zhang,Shuang Feng,Ziluo Zhang,Chuya Wang,Yongshan Ai,Yalin Xi,Lei Yin,Meiyun Shi
This study established a robust and selective ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) method to investigate the excretion behavior of polyethylene glycol 1000 (PEG1K) oligomers (N = 13–26) in rats. PEG is widely used in pharmaceutical applications, particularly in drug delivery systems, yet detailed excretion profiles of lower molecular weight PEGs remain insufficiently characterized. The developed method utilized ammonium adducts ([M+NH₄]⁺) as precursor ions in multiple reaction monitoring mode, enabling sensitive and high-throughput quantification of individual oligomers in biological matrices. Following intravenous administration in rats, excretion kinetics were monitored over 48 hours. Cumulative recovery analysis revealed that renal excretion was the dominant elimination pathway, accounting for 47.30–68.52% of the administered dose in urine, while fecal excretion represented only 0.66–3.38%. These findings provide critical insights into the in vivo disposition of PEG1K, supporting its safety evaluation and rational application in drug formulation. The presented analytical platform offers a reliable tool for polymer pharmacokinetic studies.
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高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2026
·
IF 2.8
Haiyang Cui,Dongliang Yang,Yonggang Zheng,Jing Li,Hairui Yan,Xiaoli Gao
Steroids and their metabolites play crucial roles in reproductive health, endocrine diseases, and tumor development. Comprehensive analysis of these compounds is essential for both mechanistic investigations and clinical evaluations. Although comprehensive analytical methods have been established for steroids in human clinical samples, their direct application to rat specimens remains limited, particularly with the absence of validated methods for detecting certain hydroxylated steroid metabolites in vivo. This study developed highly sensitive solid-phase extraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry methods for the quantitative analysis of 29 steroid metabolites. Through optimized derivatization of steroids and integration of two-dimensional liquid chromatography techniques, the method effectively reduces interference from non-volatile salts and overcomes trace-level detection challenges. Method validation demonstrated a wide linear range (0.002–250 ng/mL), low limits of quantification (2–100 pg/mL), high accuracy (88–114%), and precision (intra- and inter-batch CV ≤14%). The method exhibited acceptable extraction recovery, matrix effects, and stability, confirming compliance with regulatory standards. The validated method was successfully applied to characterize serum steroid metabolic profiles in both N -methyl-N-nitrosourea-induced breast cancer and ovariectomized rat models, revealing alterations in estrogen 2-hydroxylation and pregnenolone 21-hydroxylation pathways mediated by key steroidogenic enzymes, including CYP1A1/CYP1B1 and potentially CYP21A2-independent mechanisms, providing robust support for preclinical research on steroid-related diseases.
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PubMed
高影响因子
ANALYTICAL BIOCHEMISTRY
·
2023
·
IF 2.9
Yao Liu,Zhichao He,Heng Liang,Minzhen Han,Jinxingyi Wang,Qian Liu,Yanping Guan
Rapidly developing UHPLC-MS/MS bioassays with high throughput and quality are challenging yet desired in routine clinics. Methods & results A high-throughput UHPLC-MS/MS bioassay has been built for simultaneously quantifying gefitinib , ruxolitinib , dasatinib , imatinib , ibrutinib , methotrexate , cyclophosphamide and paclitaxel . After the protein precipitation with methanol, samples were separated on an Acquity BEH C 18 column following a gradient elution system with methanol and 2 mM ammonium acetate in water at 40 °C with a run time of 3 min (flow rate 0.4 mL/min). Mass quantification in the positive ion SRM mode was then performed with electrospray ionization . The method of specificity, linearity, accuracy, precision, matrix effects, recovery, stability, dilution integrity and carryover were all validated as per the guideline of the China Food and Drug Administration whose values met the admissible limits. Application of the bioassay to therapeutic drug monitoring revealed important variability in the studied anti-tumour drugs. Conclusion This validated approach was shown to be reliable and effective in clinical management, being a valuable support in therapeutic drug monitoring and subsequent individualized dosing optimization.
研究领域:
药理学
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临床医学
·
分析化学
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PubMed
高影响因子
Bioanalysis
·
2023
·
IF 1.8
Liyuan Cheng,Xiaoying Zhang,Jige Qi,Yue Zhang,Kun Zhou
Aim: To develop a UHPLC–MS/MS method for the quantification of 12 constituents in rat plasma after oral administration of Zhuanggu Guanjie. Methods: Constituent separation was performed on a C18 column, and the mass spectrometric detection was performed in multiple reaction monitoring mode with a positive–negative ionization mode. Results: The method was successfully applied to the pharmacokinetic study of these 12 constituents after rats taking Zhuanggu Guanjie capsules. The results showed that psoralen, isopsoralen and aspersaponin VI were the key effective components and had high exposure. Conclusion: A rapid, simple and sensitive ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry method for the detection of 12 components in rat plasma after taking Zhuanggu Guanjie was developed and applied in this pharmacokinetics study.
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高影响因子
PHYTOCHEMICAL ANALYSIS
·
2026
·
IF 2.9
Mengyuan Wu,Zhaojie Ji,Yanjiang Dong,Sitong Liu,Shuo Diao,Xintong Wang,Ju Zhao,Boya Zhang,Da Rong,Wenxin Xu,Enli Wang,Rui Niu,He Xiao,Mingming Yu,Zhihua Lv,Sherwin K. B. Sy,Hai Yang
Objectives This study aimed to develop and validate a UHPLC-MS/MS method for the simultaneous determination of 14 constituents related to Renshen Guben Oral Liquid (RSGB) in human plasma and to explore concentration–absolute neutrophil count (ANC) associations in cancer patients with chemoradiotherapy-induced neutropenia (CIN). Methods Candidate constituents were selected by integrating chemical representativeness, disease relevance, reference standard availability, and analytical feasibility, with support from network pharmacology. Plasma samples were collected from 25 patients before administration and at 1 and 2 h after RSGB administration. Samples were processed by liquid–liquid extraction using methyl tert-butyl ether or n-butanol and analyzed by UHPLC-MS/MS. Spearman correlation analysis was used to assess exploratory associations between post-dose concentrations of major quantifiable circulating constituents and ANC change from baseline to Day 15. Results The assay fulfilled predefined bioanalytical acceptance criteria and enabled simultaneous quantification of 14 RSGB-related constituents in human plasma. Ginsenoside Rb1 (G-Rb1), ginsenoside compound K (G-CK), and paeonol (PAE) were the major quantifiable circulating constituents, whereas protopanaxadiol (PPD) and protopanaxatriol (PPT) were only sporadically quantifiable. Exploratory analyses showed positive associations between concentrations of G-Rb1, G-CK, and PAE and ΔANC. Molecular docking provided complementary computational support for potential target interactions. Conclusions G-Rb1, G-CK, and PAE were the major quantifiable circulating RSGB-related constituents within the early sampling window, and their concentrations showed exploratory associations with ANC change. These findings provide complementary in vivo evidence for evaluating RSGB-related constituents.
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高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.1
Ruifeng Lin,Huiqiang Feng,Zhixin Zhang,Yanling Liu,Hongting Wen,Hulan Chen,Yu Fan,Yuzhu Tan,Zhentao Tang
To overcome the great challenge of simultaneously reducing the matrix effect and sensitively analyzing multi-mycotoxins in complex samples, a modified QuEChERS-UHPLC-MS/MS method based on novel nanomaterials was developed for the analysis of 18 mycotoxins in different matrices. The modified QuEChERS integrated traditional QuEChERS with freezing and magnetic dispersion solid phase extraction (MDSPE), which adopted an in-house fabricated nanomaterial (Fe 3 O 4 @MWCNT@Uio-67) as a purification material. To validate the sensitive and efficient analysis of the target mycotoxins, the established method was investigated on three medicinal and edible matrices. These matrices are typical representatives of complex and diverse matrices, of which the main ingredients are starch, oil, and polysaccharides, respectively. Under the optimized conditions, the linear detection range was 1.00–1250.00 μg/kg (R 2 > 0.998). The detection limits were down to 0.003–5.096 μg/kg. The accuracy (spiked recovery/66.38–139.17%) and precision (intra-RSDs/0.15–19.65%, inter-RSDs/0.23–16.40%) were both satisfactory. Compared to C 18 , the novel material presented a better ability to purify the substrate matrices, along with a more acceptable recovery. Through the comparison with other methods, the developed method was further demonstrated to be sensitive, efficient, and with great potential for the analysis of multi-mycotoxins in diverse and complex samples.
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高影响因子
Food & Function
·
2021
·Vol. 12
·期 24
·12683-12695
·
IF 5.396
Zhou Lu,Yat-Tin Chan,Kenneth Ka-Hei Lo,Vincy Wing-Si Wong,Yuk-Fan Ng,Shi-Ying Li,Wing-Wa Ho,Man-Sau Wong,Danyue Zhao
Dietary polyphenols are phytonutrients exhibiting multiple health benefits in humans including those in infants. However, data on breast milk (poly)phenolic composition are limited, especially among Asian populations. This study aimed to assess the levels of dietary polyphenols and their microbial-derived metabolites in the breast milk of Hong Kong lactating women, and how maternal diet correlated with the phenolic composition in breast milk. Breast milk samples from 89 healthy Hong Kong lactating women (aged 19–40 years) were collected. Maternal intake of plant-based foods and polyphenols was estimated through 3-day dietary records and the Phenol-Explorer database. Twelve commonly consumed polyphenols including their microbial-derived metabolites in breast milk were quantified using an optimized and validated UHPLC-MS/MS method. The effect of maternal intake on breast milk phenolic levels was then examined via the Pearson correlation test. The mean concentrations of individual phenolic compounds ranged from 5.1 nmol L−1 (chlorogenic acid) to 731.5 nmol L−1 (3,4-dihydroxybenzoic acid). Despite suboptimal intake of fruits and vegetables among our participants, breast milk phenolic levels were comparable to those of foreign populations. Significant correlations were found between dietary intake and multiple phenolics, particularly legume and daidzein (r = 0.33, P = 0.001), and tea and epicatechin (r = 0.30, P = 0.03). Regarding phenolic metabolites, 3,4-dihydroxyphenylacetic acid was significantly correlated with several polyphenols, particularly quercetin (r = 0.34, P = 0.002), and equol was exclusively correlated with daidzein (r = 0.46, P < 0.001). Our findings support that intake of plant-based foods significantly affects breast milk phenolic composition. Future investigation on the bioavailability and health outcomes in infants is warranted to substantiate the transferability of these bioactive phytonutrients from mother to child through lactation, and to promote maternal intake of polyphenol-rich foods.
研究领域:
营养学
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饮食科学
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分析化学
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母婴健康
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植物化学
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PubMed
高影响因子
MOLECULES
·
2020
·Vol. 25
·期 9
·2149
·
IF 3.267
Xu Yu,Fei Ma,Liangxiao Zhang,Peiwu Li
Rapeseed (Brassica napus L.) is rich in phenols, vitamins, carotenoids, and mineral elements, such as selenium. Additionally, it contains the active ingredients sulforaphane and indole-3-carbinol, which have been demonstrated to have pharmacological effects. In this study, sulforaphane and indole-3-carbinol were extracted and quantified from rapeseeds using quick, easy, cheap, effective, rugged and safe (QuEChERS) method coupled with ultra high performance liquid chromarography tandem mass spectrometry (UHPLC-MS/MS). The major parameters for extraction and purification efficiency were optimized, including the hydrolysis reaction, extraction condition and type and amount of purification adsorbents. The limit of detection (LOD) and the limit of quantification (LOQ) for sulforaphane were 0.05 μg/kg and 0.15 μg/kg, and for indole-3-carbinol were 5 μg/kg and 15 μg/kg, respectively. The developed method was used to successfully analyze fifty rapeseed samples. The QuEChERS coupled with UHPLC-MS/MS simultaneously detect sulforaphane and indole-3-carbinol in vegetable matrix and evaluate the quality and nutrition of rapeseed samples.Keywords:sulforaphane;indole-3-carbinol;QuEChERS;quantification;UHPLC-MS/MS
研究领域:
农业化学
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分析化学
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食品科学
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PubMed
高影响因子
危险品化学品经营许可证（带存储）