JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Tong Wu,Libin Pu,Wenqing Liu,Yinliang Bai,Jingjing Ma,Xia Song,Aijia Cao,Shunli Pan,Jiahui Yang,Chang Wang,Wen Qiu
Objective To develop a rapid, convenient, accurate, and low-residual-effect ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method for the determination of polymyxin B sulfate and colistin sulfate in the blood of patients with multidrug-resistant bacterial infections, as well as caspofungin acetate in the blood of patients with fungal infections, thus facilitating the rational use of antibiotics in clinical applications. Methods All analytes were diluted with 0.2 % aqueous formic acid, and plasma proteins were precipitated using acetonitrile. The selected reaction monitoring (SRM) mode was used for measurement. Separation of all analytes was completed on a Hypersil GOLD C18 column (100 × 2.1 mm, 3.0 µm). They were quantitatively analyzed using electrospray ionization on a triple quadrupole mass spectrometer in the positive ion mode. The mobile phase consisted of water (containing 0.1 % formic acid) and acetonitrile, which was delivered by gradient elution at a flow rate of 0.3 ml/min. The internal standard was bacitracin zinc (BcZn), and the column temperature was maintained at 25 °C. The runtime for each analysis was 3.5 min. Results The procedure was validated following the recommendations of the U.S. Food and Drug Administration, which included measurements of accuracy (ranging from 83.27 % to 105.86 % for within-run and between-run accuracy), precision (with coefficients of variation from 2.50 % to 16.51 % for within-run precision and between-run precision), and matrix effects (ranging from 88.65 % to 103.94 %). The extraction recoveries ranged from 38.01 % to 42.76 for polymyxin B1 (PMB1), polymyxin B2 (PMB2), polymyxin E1 (PME1), polymyxin E2 (PME2), and 88.65 % to 89.84 % for caspofungin (CPF). Plasma samples were stable under various storage conditions, including three freeze–thaw cycles at −80 °C, 24-hour periods at room temperature and 4 °C, and 30 days of freezing at both −20 °C and −80 °C, with relative standard deviations (RSD) of less than 15 %. Conclusion In this study, a UPLC–MS/MS method was developed to simultaneously quantify PMB1, PMB2, PME1, PME2, and CPF in human plasma. The method was validated in blood samples from patients with multidrug-resistant bacteria combined with fungal infections and is suitable for therapeutic drug monitoring.
研究领域:
临床药理学
·
分析化学
·
感染病学
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PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Mingyu Pan,Wenfeng Geng,Yuanxiao Wang,Makoto Tsunoda,Jiatong Liu,Yingxia Zhang,Haimei Yang,Lu-shuang Li,Shiwen Song,Jinqiang Liang,Yanting Song
Areca nuts have been used as a traditional Chinese medicine (TCM) for thousands of years. Recent studies have shown that it exhibits good pharmacological activity and toxicity. In this study, the pharmacokinetics of five major components of areca nut extract in rats were investigated using a highly sensitive ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS) method. Arecoline, arecaidine, guvacoline, guvacine, and catechin were separated and quantified accurately using gradient elution with mobile phases of (A) water containing 0.1 % formic acid-10 mM ammonium formate, and (B) methanol. The constituents were detected under a timing switch between the positive and negative ion modes using multiple reaction monitoring (MRM). Each calibration curve had a high R 2 value of >0.99. The method accuracies ranged −7.09–11.05 % and precision values were less than 14.36 %. The recovery, matrix effect, selectivity, stability, and carry-over of the method were in accordance with the relevant requirements. It was successfully applied for the investigation of the pharmacokinetics of these five constituents after oral administration of areca nut extract. Pharmacokinetic results indirectly indicated a metabolic relationship between the four areca nut alkaloids in rats. For further clarification of its pharmacodynamic basis, this study provided a theoretical reference.
研究领域:
药理学
·
分析化学
·
中药学
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DOI
PubMed
高影响因子
Thoracic Cancer
·
2023
·Vol. 14
·期 33
·3331-3341
·
IF 2.9
Mengming Xia,Xueyi Song,Zebei Lu,Yu Wang,Quan Zhou,Peiwu Geng,Shuanghu Wang,Yunfang Zhou,Qingjun Wu,Aixia Han
Background Lenvatinib is a multitargeted tyrosine kinase inhibitor used in the treatment of a variety of solid tumors. This study aims to investigate the potential pharmacokinetic interactions between lenvatinib and various azoles (ketoconazole, voriconazole, isavuconazole and posaconazole) when orally administered to rats. Methods A total of 30 Sprague–Dawley rats were randomly allocated into five groups and administered 20 mg/kg of ketoconazole, voriconazole, isavuconazole and 30 mg/kg of posaconazole and 0.5% CMC-Na, through gavage for a duration of 7 days prior to the commencement of the experiment. On the final day, the rats were given 10 mg/kg of lenvatinib. The blood concentration of lenvatinib was determined using UPLC-MS–MS. In vitro lenvatinib were incubated with azoles and rat liver microsomes (RLMs) or human liver microsomes (HLMs). Molecular docking was lastly used to examine the binding strength of the enzymes and ligands with Autodock Vina. Results AUC and C max of lenvatinib significantly increased with each of the azoles ( p < 0.05), whereas CLz/F decreased 0.83-flod, 0.41-fold ( p < 0.05) and 0.72-fold ( p < 0.01) in voriconazole, isavuconazole and ketoconazole in rats. The IC50 of lenvatinib with the azoles were 0.237, 1.300, 0.355 and 2.403 μM in RLMs and 0.160, 1.933, 3.622 and 1.831 μM in HLMs. Molecular docking analysis suggested that azoles exhibited a strong binding ability towards the target enzymes. Conclusion It is imperative to acknowledge the potential drug–drug interactions mediated by CYP3A4 between azoles and lenvatinib, as these interactions hold significant implications for their clinical utilization.
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高影响因子
Food Analytical Methods
·
2018
·Vol. 11
·期 6
·1780-1788
·
IF 2.245
Zhao Zhiyong,Yang Xianli,Zhao Xiaoyan,Chen Lei,Bai Bing,Zhou Changyan,Wang Jianhua
Fusarium species are one of the common pathogenic fungi of vegetable diseases. Some Fusarium species produce toxic secondary metabolites, which have potential health risks for humans and animals. In the study, an ultra-performance liquid chromatography tandem mass spectrometry method (UPLC-MS/MS) was developed for the analysis of 13 emerging and traditional Fusarium toxins in pepper, tomato, cucumber, and potato. Samples were extracted by a modified quick, easy, cheap, effective, rugged, and safe method. Dispersive solid-phase extraction was employed for the removal of matrix interferences from the crude extracts of various vegetables. Matrix effect was compensated using matrix-matched calibration curves. The method was fully validated according to the European Commission Decision 2002/657/EC. For all the targeted analytes, good linearity ( R 2 ≥ 0.9823) was obtained. Recoveries were in the range of 62 and 114% in pepper, tomato, cucumber, and potato, with intra-day relative standard deviations lower than 14.3%. Quantitation limits of the developed method were between 0.25 and 20 μg/kg in four sample matrices. The method was successfully employed for the analysis of Fusarium toxins in vegetable samples.
研究领域:
食品科学
·
毒理学
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高影响因子
Frontiers in Chemistry
·
2022
·
IF 5.545
Shen Qing,Wang Haixing,Quan Bin,Sun Xiuhua,Wu Guohua,Huang Darong,Wang Qingcheng,Luo Pei
Salvia miltiorrhiza Bunge (SMB) has unambiguous biological functions in cardiovascular diseases, thus has been processed into different medicine forms. However, universal analytical method for fast quantification of bioactive compounds in SMB and SMB derived products is still missing. In this study, a polarity switching strategy was developed and optimized, which enabled the detection of the target compound in both positive and negative ion modes in a single run. The MS2 features of each compound were characterized to select the most prominent transitions for quantitative and qualitative analysis. Afterwards, the performance of this method was validated in terms of linearity (≥0.9916), limit of detection (LOD, 0.003–0.135 ngml−1), limit of quantification (LOQ, 0.010–0.450 ngml−1), precision (48.23 ± 2.58 ngml−1 to 53.72 ± 3.11 ngml−1), recovery (RSD 2.04%–5.79%), and stability (RSD ≤7.52%). Finally, the bioactive compounds in SMB and SMB derived products were determined, among which salvianate A, salvianolic acid A, and rosmarinic acid were the main components in all samples. In conclusion, the polarity switching UPLC-MS/MS method is efficient in accurate determining the bioactive compounds, which greatly shorten the time for analysis when compared with conventional methods. It has great potential quality control of SMB and SMB derived products.
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PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Jing Zhao,Jingjing Pu,Xiaopeng Wu,Boyu Chen,Yan He,Yue Zhang,Bingjun Han
Matrix effect (ME) is a critical factor that can significantly compromise the accuracy of pesticide residue analyses performed using ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS). In this study, five pesticides of different types, namely difenoconazole (triazoles), chlorpyrifos (organophosphates), thiram (dithiocarbamates), carbaryl (carbamates), and pyraclostrobin (strobilurins), were selected to investigate the UPLC-MS/MS MEs in five typical tropical fruits. The MEs and possible mechanisms of the main influence factors, i.e., pH value and sugar content, were studied for the pesticide residues in the tropical fruits. The proposed method was validated in terms of linearity, limit of detection (LOD), recovery, and precision. In the range of 0.005–0.5 μg mL −1 , the coefficients of determination (r) were better than 0.999, while the LODs and recoveries ranged from 0.16 to 4.4 μg kg −1 and from 75% to 120%, respectively. Results show that among the five typical tropical fruits, the ME was largest in longan, followed by that in banana; pineapple and guava showed lower MEs than those in banana, whereas papaya had the lowest. Chlorpyrifos has the largest ME, followed by thiram and difenoconazole, and the other pesticides have very small MEs. Moreover, the MEs can be reduced by adjusting the pH value and sugar content of the sample matrix. This study can be applied to assess the influence of MEs on the analysis results.
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高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
You Long,Yuting Wang,Gan Zhang,Bei Gan,Qiang Yu,Jianhua Xie,Xinyi Zang,Yi Chen
Enniatin and Alternaria mycotoxins have presented adverse effects to food safety and human health, and an accurate, simultaneous analytical method for these mycotoxins was promising. This study reported the synthesis of a magnetic covalent organic framework (NH 2 -Fe 3 O 4 @TpBD-COF) for efficient extraction of seven mycotoxins from wheat, coupled to UPLC-MS/MS for simultaneous quantification. The magnetic solid phase extraction (MSPE) parameters, including adsorbent dose (10 mg), vortex duration (5 min), and extraction/elution solvents (ACN/MeOH, 6/4, v /v), were systematically optimized. Method validation revealed ultra-low limits of quantification (LOQs:0.03 to 0.5 μg kg −1 ), matrix effects (ME<8.49 %), recovery rates(81.3 %–109 %), and precision (RSD < 9.70). The adsorbent maintained satisfactory performance through 8 reuse cycles. Density functional theory (DFT) calculation indicated exergonic adsorption, primarily driven by hydrogen bonding, van der Waals forces, and hydrophobic interactions. The integrated method offers a sensitive and accurate approach for emerging mycotoxin analysis in wheat, potentially mitigating associated health risks.
研究领域:
食品安全
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分析化学
·
真菌毒素学
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材料科学
·
环境卫生
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PubMed
高影响因子
CURRENT DRUG METABOLISM
·
2021
·Vol. 22
·期 1
·70-82
·
IF 3.731
Zuo Lihua,Li Jia,Xue Lianping,Jia Qingquan,Li Zhuolun,Zhang Mengya,Zhao Mengfan,Wang Mengli,Kang Jian,Du Shuzhang,Sun Zhi
Background: Alpiniae oxyphyllae Fructus (AOF), a traditional Chinese medicine (TCM), is widely used in the treatment of urinary, gastrointestinal and neurologic diseases in China. Although terpenoids are the main active ingredients of AOF, there are few researches on their pharmacokinetics
and metabolism. Methods: In this study, a sensitive, rapid, accurate and novel ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was established to evaluate the pharmacokinetic behavior of five terpenoids (oxyphyllenodiol B, (4S* ,5E,10R*)-7-oxo-tri-nor-eudesm-5-en-4β-ol,
7-epi-teucrenone, (+)- (4R,5S,7R)-13-hydroxynootkatone, (E)-labda-12,14-dien-15(16)-olide-17-oic acid) in rats after oral administration of AOF extracts. 27 metabolic metabolites of the five terpenoids were identified by ultra high performance liquid chromatography -Q Exactive hybrid quadrupole-orbitrap
high-resolution accurate mass spectrometry (UHPLC-Q-Orbitrap HRMS) based on precise mass and fragment ions. Results: The established pharmacokinetic analysis method showed good linearity over a wide concentration range, and the lower quantitative limit (LLOQ) ranged from 0.97 to 4.25
ng/mL. Other validation parameters were within the acceptable range. In addition, 27 metabolites were identified in plasma, urine and feces samples, and the metabolic pathways of five terpenoids were mainly focused on glucoside conjugation, dehydration, desaturation and glycine conjugation.
Conclusion: This is the first study on the pharmacokinetics and metabolism of five terpenoids in AOF, illuminating the disposal process of terpenoids in vivo. It was expected that the results of this study would provide some references for the apprehension of the action mechanism and
the further pharmacological study of five terpenoids in AOF.
研究领域:
中药学
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分析化学
·
药理学
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高影响因子
RSC Advances
·
2026
·Vol. 16
·期 31
·28230-28242
·
IF 6.1
Jin-tuo Yin,De-mao Wang,Xue-chun Wu,Juan Lu,Zheng-ming Qian,De-qiang Li,Rui Feng
Taihangia rupestris Yu & Li (T. rupestris) was a nationally protected plant and its active compounds exhibit antidiabetic potential, but systematic phytochemical and pharmacological investigations remain limited. To balance conservation and utilization, the chemical composition and bioactivities (antioxidant and α-glucosidase inhibitory effects) of wild and cultivated T. rupestris were compared, followed by active compound screening. UPLC-MS/MS was used to identify chemical constituents in wild, mountain-cultivated, and foothill-cultivated samples, with multivariate analysis for differential components. The TFC and TPC, and the antioxidant capacity were evaluated via FRAP, CUPRAC, TRC, and DPPH assays. Additionally, α-glucosidase inhibition was assessed via IC50 determination. Online HPLC-ABTS and ultrafiltration-LC/MS (UF-LC/MS) were employed to screen antioxidants and α-glucosidase inhibitors (α-GIs), respectively, with molecular docking validating binding mechanisms. As a result, among 114 identified compounds, 111 showed significant environment-dependent variations, primarily flavonoids, phenolics, and terpenoids. Foothill-cultivated plants exhibited upregulated flavonoids/phenolics (e.g., rutin and gallic acid derivatives, P < 0.05) and superior antioxidant activity (Trolox equivalents: FRAP 367.18 ± 1.03; CUPRAC 572.40 ± 0.82) and α-glucosidase inhibition (IC50 0.2775 µg mL−1) versus wild (IC50 0.4948 µg mL−1) and mountain-cultivated samples (IC50 0.5425 µg mL−1). Ten antioxidants were screened, with seven also acting as α-GIs. UF-LC/MS and docking confirmed 8 α-GIs (binding energy < −5 kcal mol−1), where phenolic hydroxyl groups formed hydrogen bonds with ASP residues of α-glucosidase. Cultivated T. rupestris (especially foothill-grown) outperformed wild plants in bioactives composition and efficacy, serving as a sustainable alternative. Flavonoids and phenolics contributed to its antidiabetic potential via dual antioxidant and enzyme-inhibitory effects, supporting further pharmaceutical development.
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PubMed
高影响因子
CHEMICO-BIOLOGICAL INTERACTIONS
·
2026
·
IF 5.2
Peiqi Wang,Yan Chen,Jun Wu,Shiqi Jiang,Lu Cao,Ren-ai Xu,Xiaoqun Xu
Bosutinib is a second-generation tyrosine kinase inhibitor (TKI) primarily used for the treatment of chronic myeloid leukemia (CML). The aim of this study was to develop and validate a rapid and accurate ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of bosutinib and its major metabolite M5. Chromatographic separation was performed on an Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) using a gradient elution with acetonitrile and 0.1% formic acid as the mobile phase, and gefitinib was used as the internal standard (IS). Biological analysis showed that both bosutinib (2-400 ng/mL) and its metabolite M5 (1-60 ng/mL) exhibited good linearity in their respective concentration ranges, with correlation coefficients ( r 2 ) of 0.996 and 0.993, respectively. Both of them exhibited intra- and inter-day precision (RSD%) below 15% and accuracy (RE%) within ± 15%. Recoveries were all within the range of 85.3-98.0%, and matrix effects were all within the range of 91.6-101.6%. Ultimately, human liver microsomes (HLM) was used to study in vitro metabolic stability, while in vivo pharmacokinetics were evaluated in rats. In vivo pharmacokinetic studies confirmed that this method could be successfully used for the analysis of bosutinib after oral administration of 50 mg/kg in rats. In vitro results showed that bosutinib had the intrinsic clearance (CL int ) value of 0.03 mL/min/mg and the half-life (t 1/2 ) value of 79.94 min. This study provides a potential reference for the clinical investigation of bosutinib.
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高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Cuiyao He,Saisai Ling,Ying Jin,Lisha Fu,Xiaoke Dai,Xiaohui Qi,Yiying Wu,Zhenglei Wang,Yuhua Deng
Piperacillin/tazobactam and metronidazole are two commonly antimicrobials used to prevent and treat infections after liver transplantation in pediatric patients. However, under the recommended dose, it may lead to insufficient antimicrobial treatment and poor efficacy. To achieve antimicrobial therapy based on pharmacokinetic strategies, a rapid and highly sensitive ultra-high performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed to measure the plasma concentrations of piperacillin, tazobactam, and metronidazole in pediatric liver transplant recipients. Sample separation was achieved using an Acquity UPLC CSH C 18 column (2.1 × 50 mm, 1.7 μm) with gradient elution. The mobile phase consisted of ammonia solution–formic acid–water (0.5:1:1000, v / v /v) and methanol–acetonitrile (1:1, v/v). The plasma concentration range was 0.20–100.00 μg/mL, with good linear range. The intra- and inter-day precisions were less than 13.4 %, and the accuracy ranged from 90.0 % to 109.0 %. The selectivity, carryover, dilution integrity, matrix effect, recovery, and stability met the requirements of the relevant guidelines. The established UPLC–MS/MS method was successfully applied to measure the concentrations of piperacillin, tazobactam, and metronidazole in the plasma of pediatric liver transplant patients. The results showed that according to the recommended dosing regimen, piperacillin/tazobactam reached the effective therapeutic target of 50 %T > MIC in only 4 h. The maximum plasma concentration (C max ) of metronidazole ranged from 9.46 to 28 μg/mL, with an average C max of 16.59 μg/mL, which did not achieve the ideal C max /MIC ratio of 8–10.
研究领域:
临床医学
·
药理学
·
移植学
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PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 5
·e70055
·
IF 1.7
Nan Guo,Sheng Hu,Yahui Zhang,Wen Zhang,Dejun Li,Yue Tang,Zijian Tai,Xin Guo,Bing Leng
Tigecycline has been widely used for treating infections caused by multidrug resistant bacteria, but the dosage and intrapulmonary distribution were still controversial. In this study, a UPLC–MS/MS method was established and fully validated to quantify tigecycline in human plasma and BALF. A simple and rapid protein precipitation was used to extract the analytes from plasma and BALF samples. Then, tigecycline and IS were separated on a SHIMADZU AQ-C18 column and detected using electrospray ionization positive ion mode using the transitions of m / z 586.3 → 513.2 m / z for TGC and 458.0 → 441.0 m / z for minocycline (IS). The linearity of the calibration was in the range of 20–2000 ng/mL in plasma and BALF. The validated method was successfully applied to investigate pharmacokinetic characteristics of tigecycline in critically ill patients. The results suggested that after intravenous administration of 100-mg q12h tigecycline, the AUC 0–12 was 3663.02 ± 2075.84 ng × h/mL and C ss,av was 305.25 ± 172.99 ng/mL; the average plasma concentration/ELF concentration ratio was 3.66. Significant individual differences and highly variable pharmacokinetic properties were observed, indicating that adjustment of dosing regimens according to therapeutic drug monitoring is effective and efficient to guarantee the drug efficacy and safety especially for critically ill patients.
研究领域:
临床医学
·
药理学
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DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）