BIOMEDICAL CHROMATOGRAPHY
·
2024
·Vol. 38
·期 12
·e6034
·
IF 1.8
Feng Chen,Huanhuan Li,Xiaoxia Yang,Ziwei Deng,Hongqiang Wang,Zhihua Shi,Chengfeng Qiu
To facilitate clinical therapeutic drug monitoring (TDM) of polymyxin B (PB) and polymyxin E (PE), we developed and validated a simple LC–MS/MS method for simultaneous determination of PB (including polymyxin B1 (PB1), polymyxin B2 (PB2), polymyxin B3 (PB3) and isoleucine-polymyxin B1 (ile-PB1)) and PE (including polymyxin E1 (PE1) and polymyxin E2 (PE2)) in human plasma. PB or PE was extracted from 20.0 μL plasma using a 5% (v/v) formic acid acetonitrile solution and separated on a BEH-C18 column (2.1 × 100 mm, 1.7 μm) with a mobile phase consisting of 0.8% formic acid aqueous solution and 0.2% formic acid acetonitrile solution. Gradient elution was performed over 5.5 min at a flow rate of 0.250 mL/min. Quantitative analysis was conducted in positive ion scanning mode by electrospray ionization and multiple reaction monitoring. The method validation was conducted based on bioanalytical method validation guidance, including specificity, calibration curve, precision, accuracy, recovery, matrix effect, stability and dilution integrity and all of the results satisfied the requirements. The method was simple, robust and high-throughput and is currently being used to provide a TDM service to enhancing therapeutic efficacy and safety use of the PB and PE.
研究领域:
分析化学
·
临床医学
·
药理学
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DOI
PubMed
高影响因子
Analytical Methods
·
2014
·Vol. 6
·期 9
·2998-3008
·
IF 1.938
Guanghui Liu,Wei He,Hao Cai,Xiuman Sun,Waner Hou,Manna Lin,Zhiyong Xie,Qiongfeng Liao
A rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed to simultaneously determine berberine, palmatine, coptisine, epiberberine and jatrorrhizine in rat plasma, using tetrahydropalmatine as an internal standard. The separation of the five compounds was carried out on a C18 column using a mobile phase consisting of acetonitrile and water (containing 5 mmol ammonium acetate adjusted to pH 5.0 with formic acid). The detection was performed in the multiple reaction monitoring (MRM) mode via the electrospray ionization (ESI) source operating in the positive ionization mode. Linear calibration curves were obtained over the concentration range of 0.20–200.0 ng ml−1 for berberine, and 0.20–100.0 ng ml−1 for palmatine, coptisine, epiberberine and jatrorrhizine. The accuracy, precision and extraction recovery of the five analytes were all satisfactory. The validated method was successfully applied to study the pharmacokinetic differences of the five protoberberine-type alkaloids after the oral administration of Rhizoma coptidis (RC) and Jiao-Tai-Wan (JTW) extract. It was found that the Tmax values of the five ingredients in the JTW extract were significantly increased (P < 0.05) when compared with those in RC. In addition, the AUC0–t of palmatine, coptisine and epiberberine were significantly increased (P < 0.05).
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高影响因子
Marine Drugs
·
2026
·Vol. 24
·期 6
·215
·
IF 5.7
Xiaochen Niu,Jun Zhao,Deqi Ding,Wei He,Guanhua Du,Jiejie Hao,Jianchun Zhao
LY104 (previously designated as B7) is a selective phosphodiesterase 4 inhibitor with promising activity against chronic obstructive pulmonary disease. We previously reported its single-dose pharmacokinetics and tissue distribution in rats. In the present study, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the simultaneous quantification of LY104 and its major metabolite M1 in rat plasma following ICH M10 guidelines. The method showed excellent linearity over 20–1200 ng/mL for both analytes, with retention times of 2.85 min (LY104) and 3.22 min (M1). Using this method, we extended our previous work in several directions. Re-analysis of previously published single-dose pharmacokinetic and tissue distribution data revealed no significant sex differences for LY104. Newly generated multiple-dose studies (1 mg/kg daily for 7 days) demonstrated no accumulation of LY104 or M1. The pharmacokinetic profile of M1 was quantified for the first time. Comprehensive in vitro investigations included plasma and liver microsomal stability, plasma protein binding, and excretion studies. This systematic preclinical pharmacokinetic characterization of LY104 and M1, incorporating re-analysis of existing data with sex stratification, newly generated multiple-dose and metabolite data, excretion studies, and comprehensive in vitro investigations, provides useful information to support further drug development and clinical trial design.
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2018
·
IF 2.746
Guihua Gao,Yanyan Xing,Tingting Liu,Jian Wang,Xiaohong Hou
Four water stable metal-organic frameworks (MOFs), MIL-101(Cr), MIL-100(Fe), MIL-53(Al), and UiO-66(Zr), were used as adsorbents for concentration of four androgens and progestogens from water. The adsorption abilities of target analytes on the four MOFs were investigated by experimental and molecular simulation strategies, and UiO-66(Zr) was ultimately selected as the sorbent to develop a porous membrane protected micro-solid-phase extraction (μ-SPE) method for simultaneous extraction androgens and progestogens in environmental water samples followed by LC-MS/MS detection. Several variables affecting the extraction efficiency were systematically investigated, including pH, salt concentration, extraction time, kind of desorption solvent, and desorption time. Under the optimized conditions, excellent linearity was obtained in the range of 20.32–2032 ng/L for T, 10.24–1024 ng/L for P, 7.624–762.4 ng/L for TP , and 8.376–837.6 ng/L for MPA . Limits of detection (LODs) and limits of quantification (LOQs) were 10 ng/L and 20 ng/L for T, 4.0 ng/L and 10 ng/L for P, 2.0 ng/L and 7.0 ng/L for TP, and 3.0 ng/L and 8.0 ng/L for MPA, respectively. The recoveries were ranged from 80.5% to 102.4%. Furthermore, the μ-SPE device could be used for at least 10 extractions (RSD < 10.0%). Meanwhile, comparison was made with solid-phase extraction, and the developed method was demonstrated to be a convenient and eco-friendly pretreatment method for water samples.
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高影响因子
RSC Advances
·
2017
·Vol. 7
·期 69
·43621-43635
·
IF 3.108
Huanyu Guan,Xiaoming Wang,Shiping Wang,Yang He,Jiajing Yue,Shanggao Liao,Yuanda Huang,Yue Shi
Shengjiang Xiexin decoction (SXD) exerts protective effects against gastrointestinal injury induced by irinotecan hydrochloride (CPT-11). The intestinal bacteria-associated in vitro pharmacokinetics of 16 components of SXD in normal rats and those with CPT-11-induced gastrointestinal toxicity were compared in this study. A sensitive and reproducible ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) method was developed for the quantification of 16 components of SXD in a rat intestinal bacteria incubation system, using naringin, naringenin and tetrahydropalmatine as internal standards (ISs). The samples were prepared via salting-out assisted liquid–liquid extraction (SALLE) with NaCl to reduce matrix effects. Chromatographic separation was performed on a sub-2 μm analytical column with acetonitrile and 0.1% aqueous formic acid as mobile phase. All of the analyzed components and ISs were detected via multiple reaction monitoring (MRM) scanning with electrospray ionization. The proposed method was successfully applied for the in vitro pharmacokinetic analysis of the multiple components of a complex mixture consisting of a traditional Chinese medicine (TCM) and an intestinal bacterial incubation system. The pharmacokinetic parameters of some flavonoid glycosides and aglycones in the rats with CPT-11-induced gastrointestinal toxicity were significantly different (p < 0.05, p < 0.01) from those in the normal rats, which suggested that consumption of CPT-11 could qualitatively and/or quantitatively alter the intestinal bacteria as well as the metabolic activities of enzymes. The in vitro pharmacokinetic analysis of these components in the intestinal bacterial incubation system provided valuable information for achieving a deeper understanding of the mechanisms involved in the alteration of intestinal bacteria induced by CPT-11 and further in vivo pharmacokinetic research on SXD. The intestinal bacteria-based pharmacokinetic method could benefit the study of interactions between TCMs and chemical drugs in clinical use.
研究领域:
药理学
·
中药学
·
胃肠病学
·
分析化学
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DOI
高影响因子
PHYTOMEDICINE
·
2022
·
IF 6.656
Yu Du,Chang Li,Shouchao Xu,Jiehong Yang,Haitong Wan,Yu He
Background Astragali Radix-Safflower combination (ARSC) is widely utilized in clinic to treat cerebral ischemia/reperfusion injury (CI/RI). Whereas, there is no in-depth research of the pharmacokinetics (PK) and pharmacodynamics (PD) analysis of ARSC after intragastric administration in rats with CI/RI. Purpose The purpose of this research is to investigate the PK characteristics of eight active ingredients (astragaloside IV, calycosin , calycosin-7-O-β-glucoside, formononetin , ononin , hydroxysafflor yellow A, syringin and vernine) of ARSC, and the regulation of neurotransmitters disorders, revealing the pharmacodynamic substance basis and the mechanism of ARSC in treating CI/RI from the molecular level. Methods We established a new method which based on blood-brain dual channel microdialysis (MD) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) to continuously gather, and determine the components of ARSC and neurotransmitters related to CI/RI in vivo . The collected data were analyzed by sigmoid-E max function. The neurotransmitters primarily regulated in CI/RI rat were discussed by principal component analysis and the compound most associated with total pharmacodynamics was chosen by partial least squares regression . Results The validated LC-MS/MS method had specificity and selectivity to simultaneously analyze the concentration of eight active components of ARSC extract and five neurotransmitters of CI/RI rats. The recovery rates of brain MD probe and blood MD probe were stable within six hours. The MD probes recovery rates decreased with the increase of flow rates, but the solution concentration had little effect on the probes recovery rates. It was feasible to correct the recovery rates of probes in vivo by using reverse dialysis method. All eight active ingredients of ARSC could pass across the blood brain barrier after CI/RI. ARSC regulated the release of glutamate (Glu), γ-aminobutyric acid (GABA), dopamine (DA), 5-hydroxytryptamine (5-HT) and aspartic acid (Asp). Notably, astragaloside IV and hydroxysafflor yellow A might have better regulatory effect on neurotransmitters in comparison with other six measured components of ARSC, and Glu was the neurotransmitter mainly regulated in CI/RI rats. Conclusion The ARSC was able to treat CI/RI through ameliorating neurotransmitters disorders. There was a hysteresis between the peaked drug concentration and maximum therapeutic effect of ARSC. The drug effective concentrations range of ASIV, calycosin, calycosin-7-O-β-glucoside, syringin and vernine in blood microdialysate and calycosin, syringin, vernine in brain microdialysate were narrow, which need be paid attention in clinical use.
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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
Yufeng Ni,Chenxin Ding,Minlu Cheng,Li Ding
The use of conventional opioids that act on μ-receptors is a recognized care agent for moderate-to-severe acute treatment. However, recent attention has shifted to a new class of μ-receptor agonists which can selectively activate the G-protein pathway and thus have better efficacy and fewer side effects. Recently, YZJ-4729 was developed as a new G protein selective μ-opioid receptor agonist. And for its clinical trial investigation usage, a rapid LC-MS/MS method was established for the concurrent measurement of YZJ-4729 and its major metabolite M10 in human plasma. A step involving the precipitation of proteins was used for plasma sample preparation. The chromatography separation was done on a Poroshell 120 EC-C18 analytical column (2.1 × 50 mm, 2.7-μm, Agilent). Gradient elution was performed with 5.0 mM ammonium acetate (NH 4 Ac) and 0.1 % formic acid (FA) water solution as the mobile phase A and pure acetonitrile (ACN) as the mobile phase B. Detection occurred in the mode of positive ion electrospray ionization through multiple reaction monitoring using deuterium YZJ-4729 (d6-YZJ-4729) as the internal standard. The ionic transitions used were YZJ-4729: m/z 409.3 → 244.2; d6-YZJ-4729: m/z 415.3 → 244.2; M10: m/z 425.3 → 260.2;). The method showed excellent linearity across the ranges of 0.500 to 500 ng/mL for YZJ-4729 and 0.0500 to 50.0 ng/mL for M10. The method was utilized to assess the plasma concentrations of YZJ-4729 and M10 in healthy volunteers after a 30-min intravenous infusion in the phase I clinical study, and the clinical pharmacokinetic profiles of YZJ-4729 and M10 were described.
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DOI
PubMed
高影响因子
Journal of Functional Foods
·
2024
·
IF 3.8
Yanmei Li,Longjian Zhou,Qiuyu Xia,Yingying Nie,Zeyuan Ma,Yayue Liu,Zhiyou Yang,Pengzhi Hong,Yi Zhang
Functional foods are prospective in improving memory decline caused by Alzheimer’s disease and aging. The Edible seaweed Hizikia fusiforme functional oil (HFFO) inhibited acetylcholinesterase, prevented cellular neuroinflammation, and improved memory deficits in zebrafish models in the previous studies. To realize its greener preparation and lipid oxidation mitigation and study its effects on higher animals, more investigations are necessary. Herein, sub-critical fluid extraction of HFFO and successive complex coacervation embedding yielded a water-soluble and anti-oxidative microcapsule HFFOM, which displayed in vivo memory-improving effects on LPS-injured zebrafish and normal rodents in different behavior tests. HFFOM can elevate the level of the neurotransmitter acetylcholine while decreasing the levels of MDA, IL-1β, and TNF-α in the zebrafish brain. LC-MS/MS and lipidomic analysis suggested its predominant memory-improving ingredients to be linolenic, erucic, nervonic, arachidonic, linoleic, eicosatrienoic, docosahexaenoic, and docosapentaenoic acids. This study enlightens the potential of HFFOM in developing memory-enhancing functional foods or drugs.
研究领域:
药理学
·
神经科学
·
食品科学
·
生物化学
·
生物技术
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高影响因子
危险品化学品经营许可证（带存储）