ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2026
·
IF 3.8
Wang Dong,Li Mengrong,Zhang Xiangyu,Chai Shiwei,Chen Di
A novel ultrasound-assisted magnetic sorbent–wrapped stick dip extraction (UA-MSWS-DE) method was developed for the batch-scale determination of seven tyrosine kinase inhibitors (TKIs) in human plasma. The extraction device was fabricated by immobilizing octadecylphosphonic acid–functionalized magnetic nanoparticles onto flame-sealed glass capillaries embedded with magnets. Ultrasonic-assisted dip extraction was used to extract TKIs from diluted plasma, followed by quantification via liquid chromatography–tandem mass spectrometry (LC-MS/MS). Key extraction parameters were systematically optimized, yielding the following optimal conditions: sample pH 5.0 and volume 1.0 mL, sorbent particle size 20 nm and dosage 10 mg, extraction time 20 min, and desorption with 150 µL of ethanol for 8 min. The method demonstrated excellent linearity ( R 2 ≥ 0.99), low limits of quantification (0.1–5.0 ng/mL), and good intra-/inter-day precision (RSDs < 14.95%). The accuracy in blinded plasma samples, tested at 0.25–25% of the studied concentration range, ranged from 87.13 to 112.33%. Compared to conventional magnetic dispersive solid-phase extraction, the UA-MSWS-DE strategy simplifies handling and is designed to facilitate potential parallel processing using only an ultrasonic bath. Five greenness metrics confirmed the method’s high sustainability. Furthermore, the modular design enables adaptation to other analytes by modifying the sorbent coating, making UA-MSWS-DE a sensitive, green, and automation-ready method for therapeutic drug monitoring. Graphical
✓ 已验证
产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 12
·e4373
·
IF 1.688
Qi Wen,Hai-Long Li,Feng Chen,Jing-Wen Gong,Wei-Wei Guan,Nai-Guang Fu,Yin-Feng Tan
The aim of the present study was to develop a rapid, specific and sensitive LC–MS/MS method for the determination of DPHB [7-(4″-hydroxy-3″-methoxyphenyl)-1-phenyl-4-hepten-3-one] in rat plasma using yakuchinone A as an internal standard (IS). n -Hexane was used for the extraction of DPHB from rat plasma. Chromatographic separation of DPHB was achieved using a Kinetex XB-C 18 column (2.10 × 50 mm, 2.6 μm) at 40°C. The mobile phase consisted of water (containing 0.1‰ formic acid, A) and acetonitrile (containing 0.1‰ formic acid, B) under a gradient elution at a flow rate of 0.3 mL min −1 . Positive electrospray ionization and multiple reaction monitoring mode were used for detection. The selected precursor ion to product ion pairs, m / z 311.3 → 137.0 for DPHB and m / z 313.1 → 137.0 for yakuchinone A, were monitored. Good linearity was observed over the concentration range from 2 to 2000 ng mL −1 ( r = 0.9969). The recovery efficiency of DPHB from rat plasma was 54.8–69.7%, while the matrix effect ranged from 99.7 to 113%. Intra- and inter-day precision and accuracy values were within ±15% at three different quality control concentration levels. This validated method was successfully applied to pharmacokinetic studies in rats after a single p.o. or i.v. dose of DPHB solution. The route of administration significantly influenced systemic exposure to DPHB, and low bioavailability of DPHB was observed. The method developed here will be further improved and used in future pharmacokinetic studies.
研究领域:
分析化学
·
药学
·
药代动力学
·
生物分析
✓ 已验证
DOI
高影响因子
FOOD CHEMISTRY
·
2026
·
IF 10.4
Xia Xu,Chen Liang,Zengbo Fang,Ting Zhao,Mingjie Liu,Yan Cui
A novel chiral derivatization reagent {DMT-OTZD-3( S )-Apy} was synthesized. • A sensitive LC-MS/MS method was developed for the simultaneous determination of six NSAID enantiomers. • Determination of NSAID enantiomers was carried out firstly in multi-specie meat products. In stock farming, illegal use of non-steroidal anti-inflammatory drugs has caused food safety problems. A novel chiral derivatization reagent targeted carboxyl groups, ( S )-[(( R )-1-(4,6-dimethoxy-1,3,5-triazine-2-yl)-2-oxothiazolidine-4‑carbonyl] pyroli-dine-3-amine {DMT-OTZD-3( S )-Apy}, was synthesized. After derivatization with it, the first multi-residue and simultaneous determination targeted six NSAID enantiomers in beef and mutton products was conducted. The method was validated to be selective, and got an excellent linear relationship for all enantiomers within their respective concentration ranges ( r 2 ≥ 0.9990). The average recoveries were from 91.7% to 104.3%, and the RSDs corresponding to intra-day and inter-day precision did not exceed 6.2%. The limit of detections spanned the interval of 0.30–1.42 ng/g, which were far lower than maximum residue limits established by China and the European Union. The method would provide methodology support for the risk assessment of NSAIDs in meat products from enantiomeric levels. Download: Download high-res image (122KB) Download: Download full-size image
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Bingqing Zhang,Xueyong Li,Yiying Chen,Bo Chen,Yu Cheng,Hailing Lin,Wancai Que,Maobai Liu,Lili Zhou,Hui Zhang,Hongqiang Qiu,Chaoyang Wu
Polymyxin B (PB) is currently one of the last resort treatment options against carbapenem-resistant gram-negative bacterial pathogens. Pharmacokinetics/pharmacodynamics (PK/PD) guided therapeutic drug monitoring (TDM) of antibiotics is critical for optimizing dosage regimens to maximize efficacy, minimize toxicity, and delay the emergence of resistance. Currently, methods for determining PB in human plasma and epithelial lining fluid (ELF) are limited. In this study, we developed and validated a simple method for PB determination in human plasma and ELF using LC-MS/MS. Protein precipitation of the sample was conducted with 0.1% formic acid-acetonitrile. Polymyxin B1 and B2 were separated on a C 18 column and detected within 4 min by the mass spectrometer in the positive mode coupled with multiple reaction monitoring. The calibration curve range was 0.156–10.0 and 0.0156–1.00 μg/mL in the plasma for polymyxin B1 and B2, respectively, and was 0.0625–2.00 and 0.00625–0.200 μg/mL for polymyxin B1 and B2, respectively in bronchoalveolar lavage fluid. The accuracy of the intra- and inter-assay studies ranged from 80.6% to 114.9%, and the coefficients of variation for intra- and inter-day assays were less than 14.8%. Among a considerable number of patients, the average steady-state plasma concentration of PB was suboptimal. Moreover, the exposure to PB in patients with acute kidney injury (AKI) was considerably higher than that in patients without AKI. Meanwhile, a higher concentration of PB in ELF could be achieved than that in plasma after PB nebulization treatment. The established method was proven to be rapid, simple, and suitable for TDM of PB and PK/PD studies in human plasma and ELF.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Si-Tao Xu,Hao-Wen Jin,Xin Jin,Bi-Xin Xu,Yu Zhang,Tao Xie,Guangji Wang,Jiankun Wang,Le Zhen
VK2809 is a promising drug candidate in Phase II clinical trials for the treatment of non-alcoholic steatohepatitis (NASH). It is a prodrug with a HepDirect strategy, which can achieve selective hepatic metabolic activation , generating an active metabolite VK2809A as a potent and selective agonist for thyroid hormone receptor beta (TRβ), a concomitant reactive metabolite VK2809B, and a glutathione (GSH) conjugate MB06588. Currently, there is no convenient and sensitive bioanalytical method for the simultaneous determination of the above three metabolites. Herein, we established an LC-MS/MS method to separate VK2809 and its metabolites on the XSelect HSS T3 column and quantified them in negative electrospray ionization mode. Subsequently, several factors were investigated such as the use of 60% acetonitrile for homogenization to stabilize the analytes, the addition of 20 mM glutathione for the derivation of VK2809B, and the protein precipitation with methanol containing Sobetirome as the internal standard (IS). The method exhibited good linearity for all compounds (19.4–388.4 nM for VK2809; 27.4–2744.4 nM for VK2809A and 10.6–211.0 nM for MB06588) with great correlation coefficients (r > 0.996). The method validation also demonstrated acceptable precision (RSD < 13.0% for VK2809, RSD < 7.9% for VK2809A, RSD < 14.4% for MB06588) and accuracy (92.7%−103% for VK2809, 91.2%−107.3% for VK2809A, 96%−106.7% for MB06588). The matrix effect, recovery, and stability were also suitable to determine all the analytes. This method is suitable for the bioanalysis of VK2809 and its metabolites and has been successfully applied to the study of intrahepatic exposure in rats. It is expected to be further practiced in drug design , optimization, and metabolism study in the following research.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Huanhuan Yang,Cong Liu,Chuanhong Zhu,Yan Zheng,Juan Li,Qianyun Zhu,Hao Wang,Xiangming Fang,Quan Liu,Man Liang,Zilong Liu
Determination of antipsychotics from biological samples is meaningful in the field of clinical and forensic medicine. Compared to blood, keratinized matrices such as hair and nails have attracted increasing attention in drug analysis for wider detection window. Nevertheless, the distribution and stability of antipsychotics in keratinized matrices are not clarified yet. Therefore, we developed a LC-MS/MS based method for simultaneous determination of 10 antipsychotics from blood, hair and nails, with high recovery (78.1–107.4%, 71.3–93.5% and 75.2–90.5%), low LOD (5–10 pg/mL, 5–10 pg/mg and 5 pg/mg) and high accuracy (96.0%−101.6%, 97.5%−102.5% and 97.6–101.7%). The method was applied to sets of blood, hair, and nail samples of 54 patients who received long-term therapy, and significant correlations between drug concentrations in blood and hair was found, while the correlation between nails and other matrices varied depending on the drug. Except for olanzapine , the concentrations of antipsychotics in segmental hair samples were consistent with drug exposure. Besides, the hair and nail samples of suspects in two forensic cases were analyzed and provided supporting evidence for the suspects’ psychiatric state. Our research offered a deeper understanding of keratinized matrix as stable and retrospective bio-samples for antipsychotics detection in forensic practice.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CHROMATOGRAPHIA
·
2023
·Vol. 86
·期 8
·595-603
·
IF 1.7
Huang Dan,Tian Yufei,Zheng Yili,Li Mengyu,Xu Xia,Chen Hongyuan,Rui Wen
Forced degradation studies aim to systemically characterize the degradation products of an active pharmaceutical ingredient (API) and its formulations under harsh conditions that accelerate degradation. These studies are especially valuable for sustained-release products in selecting appropriate packaging materials and storage conditions in the field of pharmaceutics. To demonstrate the degradation pathways and degradation products of the API and products, mass spectrometry is used for further characterization of the degradation products. Goserelin acetate sustained-release implant, which is prepared by hot melt extrusion using biodegradable material polylactic acid-glycolic acid copolymer as a carrier, is used for the treatment of early breast cancer in premenopausal and perimenopausal women. In this study, a simple and sensitive high-performance chromatography method was established following the ICH guidance. We conducted forced degradation experiments to determine the conditions of the product. The forced degradation studies of the goserelin acetate sustained-release implant showed the presence of a single impurity during thermal degradation, as observed in the HPLC analysis. To elucidate the structure of the impurity and characterize its degradation pathway, we performed further characterization using LC–MS.
✓ 已验证
产品关联
DOI
高影响因子
CHROMATOGRAPHIA
·
2022
·Vol. 85
·期 3
·221-231
·
IF 2.213
Sun Zhiping,He Lingli,Yang Qingqing,Zhang Haizhi,Xu Weiren,Qin Xinguang,Liu Gang,Hu Zhongze,Zhang Luyong,Liu Changxiao
The influence of genetic polymorphism of metabolic enzymes on drug–drug interactions (DDI) should be thoroughly investigated owing to its remarkable effect on therapeutic treatments that are futile. Here, different from earlier articles focused on various CYP subfamilies and their isoforms, the effect of genetic polymorphs of a particular isoform, CYP2C9, was comprehensively studied. Using diclofenac as probe substrate, the influence of three CYP2C9 variants (CYP2C9*1, *2 and *3) on DDI was conducted from the measurement of inhibitory ability of six drugs towards three variants. A modified LC–MS/MS method according to former report was constructed for the determination of 4ʹ-hydroxydiclofenac in CYP2C9 enzyme incubation system and validated for accuracy, precision, linearity range within the acceptance criteria for regulatory guidelines. After selecting appropriate incubation time and enzyme concentration, the kinetic parameters of three CYP2C9 variants towards diclofenac were examined and half inhibitory concentrations (IC 50 ) of six drugs towards three CYP2C9 variants were determined. IC 50 of paroxetine and losartan towards CYP2C9*2 were almost threefold higher and 2.5-fold lower than that towards CYP2C9*1, respectively. IC 50 of glibenclamide towards CYP2C9*3 was twofold more than that towards CYP2C9*1. Our results could offer effective guidelines for co-administration of these six drugs with various CYP2C9 substrates in individuals carrying variant CYP2C9 alleles, also broaden the application area of LC–MS/MS.
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Quancheng Yang,Peng Cao,Yi Lv,Hua Peng,Xuejia Zhai
Pediatric heart failure (HF) is an important clinical disease with high hospitalization rates, morbidity, mortality and medical costs. Sacubitril/valsartan (also known as Entresto), was approved for the treatment of adult HF and is recently used in pediatrics. However, clinical therapy on children is more challenging than adults, and the pharmacokinetics of Entresto in children are still largely unknown and urgently needed. Herein, we aim to develop a simple and sensitive analytic method to monitor Entresto in pediatric patients, which is of great importance for individualized safe medication in children. Specifically, a liquid chromatography tandem mass spectrometry method for simultaneously quantification of valsartan, sacubitril and its bio-active metabolite sacubitrilat in human plasma has been developed and validated in pediatric patients. Plasma samples were pretreated with acetonitrile for protein precipitation. Elution was performed on X Select HSS T3 column (2.1 × 100 mm, 5 µm; Waters) column using an isocratic mobile phase process consisting of 0.1% formic acid aqueous solution and 0.1% formic acid acetonit rile with a total run time of 3.0 min. Valsartan-d3, sacubitrilin-d4 and sacubitrilat-d4 were used as the corresponding deuterium internal standards. According to the Bioanalytical Method Validation Guidance for Industry, the method was validated in the range of 0.5–5000 ng/mL. Intra- and inter-day accuracy of sacubitril,valsartan and sacubitrilat ranged from 93%− 108%, 98%− 109%, 91%− 102%, respectively, with relative standard deviation of precision ranging from 2.0% to 5.1%, 2.4%− 7.5%, 1,3%− 7.4%. The proposed method demonstrated good accuracy, precision and linearity. The matrix factors normalized by internal standard meet the acceptance criteria. The method was fully validated and applied in 39 children. Trough concentration of the three substances to be measured were: valsartan (11.3–938.0 ng/mL), sacubitril (0.5–395.5 ng/mL) and sacubitrilat (522.1–4890.0 ng/mL). Overall, this is the first study to simultaneously determined the plasma valsartan, sacubitril and sacubitrilat concentrations in children, which is believed to facilitate the clinical management of pediatric HF.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2023
·Vol. 37
·期 12
·e5751
·
IF 1.8
Feng Chen,Xiaoxia Yang,Huanhuan Li,Xiaodan Zeng,Ziwei Deng,Hongqiang Wang,Yuanxiang Jin,Chengfeng Qiu,Zhihua Shi
In order to facilitate therapeutic drug monitoring of tacrolimus and cyclosporine A in clinical practice, a simple, rapid, robust, sensitive and specific LC–MS/MS assay was developed and validated for the simultaneous determination of tacrolimus and cyclosporine A in human whole blood. Erythrocytes were destroyed using internal standard solution with 10% (w/v) zinc sulfate in water. The analytes were extracted from 100 μl of whole blood by protein precipitation with acetonitrile. Chromatographic separation was conducted on a Kinetex PFP column (60°C) by a gradient elution with a flow rate of 0.450 ml/min in 2.5 min. Quantitative analysis was performed using electrospray ionization and multiple reaction monitoring in positive ionization mode. The method was fully validated as per current guidelines on bioanalytical methodologies of the US Food and Drug Administration and European Medicines Agency. The method developed was applied successfully in analyzing clinical samples from patients administered tacrolimus or cyclosporine A. The sample treatment procedure was rationalized and improved to fulfill the complete target extraction. The chromatography conditions were optimized to achieve rapid and accurate quantification of both analytes. This method may be beneficial as a constructive input for the therapeutic drug monitoring of tacrolimus and cyclosporine A in obtaining individualized therapy.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Jiayi Sun,Jinna Dai,Xingqi Wang,Hong Shang
The objective of this study is to develop a quick and precise chiral liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) technology that operates in reversed phase mode. Following oral administration of 5.0 mg/kg rac -pranoprofen, the suggested approach was completely validated and successfully used to the stereoselective detection of pranoprofen enantiomers in rat plasma for the first time. Both the polysaccharide derivatized chiral stationary phase and a homemade β-cyclodextrin (β-CD) derivatized based chiral column were assessed. The latter one, a per-4-chlorophenylcarbamate-β-cyclodextrin bonded chiral stationary phase (CPCDP) made in our laboratory, allowed for the highly sensitive detection, relatively short retention time and complete separation (resolution 2.0) of the pranoprofen enantiomers. A solid phase extraction (SPE) procedure on C 18 cartridge was optimized for the extraction of S -(+)-, R -(−)-pranoprofen and internal standard ( S -(+)-ketoprofen, IS) from rat plasma in detail. Acetonitrile with 0.1 % formic acid in aqueous phase (60:40, v:v ) at a flow rate of 0.6 mL/min was the ideal mobile phase condition. The outcome of pharmacokinetic study showed that the values of maximum plasma concentration (C max ) and the area under plasma drug concentration–time curve to infinity (AUC 0-∞ ) for S -(+)-pranoprofen were 1.79 and 1.90 times greater than R -(−)-isomer, respectively. Altogether, this work is the first to examine the stereospecific pharmacokinetics of pranoprofen enantiomers in vivo , whose data provided potential possibility for the development of pure isomer with superior pharmacological activity and safety to replace racemic application in the clinic.
✓ 已验证
产品关联
DOI
高影响因子
FOOD AND AGRICULTURAL IMMUNOLOGY
·
2021
·
IF 3.101
Jie-Biao Guo,Tai-Long Wei,Qing-Hua He,Jin-Sheng Cheng,Xiu-Zhen Qiu,Wang-Pei Liu,Xian-Quan Lan,Lu-Fen Chen,Min Guo
A magnetic separation-based immunosensor for deoxynivalenol assay, coupled with a nano-affinity cleaning up for instrumental confirmation, was developed. Maltose-binding protein with mimic epitope of DON was coupled to CdSe/ZnS quantum dot nanobeads for fluorescent reporter. Graphene oxide was linked with magnetic nanoparticles and protein G for immunomagnetic adsorbent. The magnetic separation of reporter could be inhibited by DON so the fluorescent remained in the solution indicates a good quantitative correlation to DON concentration. The DON separated by immune adsorbent can be cleaned up for instrumental confirmation. The optimized immunosensor showed results as follows: the linear range was in 0.3–3000 ng mL−1. The limits of detection (S/N = 3) were 0.50, 1.0, and 3.0 ng mL−1 in different backgrounds. The recoveries for DON-spiked samples range from 78.7% to 88.5%. Both results of UPLC-MS/MS based on affinity column purification and coupled with nano-affinity cleaning up showed a good agreement with the current immunosensor.
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）