Current Pharmaceutical Analysis
·
2021
·Vol. 17
·期 10
·1249-1256
·
IF 0.89
Sun Qian,Yang Yu-fei,Zou Qiao-gen,Xia Yun-yan,Han Cheng-qun
Background: A liquid chromatography-tandem mass spectrometric (LC-MS/MS) method had been developed for the quantification of acotiamide in rat plasma and been applied to pharmacokinetic studies. However, there was no LC-MS/MS method been developed for the determination of acotiamide
in human plasma and its pharmacokinetic study. Objective: A simple and fast LC-MS/MS method was established and validated for the quantification of acotiamide in human Received: plasma and was applied to a pharmacokinetic study. Methods: Sample preparation was accomplished Revised:
Accepted: through protein precipitation, and chromatographic separation was achieved on a Welch, Ultimate XB-C18 column (2.1×50 mm, 3 μm) with a security guard cartridge C18 using a binary gradient with DOI: mobile phase A (Methanol) and B (the solution of 10 mM Ammonium acetate with
0.1% Formic acid) at a flow rate of 400 μL/min. Results: The retention time of acotiamide and its internal standard, acotiamide-d6 was 1.78 min and 1.79 min, respectively. The total run time was 4.0 min. The method was developed and validated over the concentration range of 0.500-100
ng/mL for acotiamide, with correlation coefficient greater than 0.9987. The extraction recovery was more than 108.43% and the matrix effect was not significant. The inter- and intra-day precisions were below 5.80% and accuracies ranged from 92.7 to 103.0%. Acotiamide was demonstrated to be
stable in human plasma under the tested conditions. Conclusion: The validated LC-MS/MS method was successfully applied to study the pharmacokinetic profiles of acotiamide in human plasma after oral administration and has achieved satisfactory results.
研究领域:
药物分析
·
临床药理学
✓ 已验证
DOI
高影响因子
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
·
2023
·Vol. 24
·期 18
·13751
·
IF 5.6
Hsin-Hua Liang,Yu-Chao Lin,Chin-Chuan Hung,Yu-Chi Hou,Yi-Hui Lin
In this study, we established a novel capillary electrophoresis method for monitoring the concentration of doripenem in human plasma. As a time-dependent antibiotic, doripenem maximizes its antibacterial effects and minimizes the potential for antibiotic resistance through careful therapeutic drug monitoring. Two online preconcentration techniques, field-enhanced sample stacking (FESS) and sweeping, were coupled to enhance the detection sensitivity. Briefly, an uncoated fused silica capillary (40 cm × 50 μm i.d) was rinsed with a high conductivity buffer (HCB) composed of 150 mM phosphate buffer (NaH2PO4, pH 2.5) and 20% methanol. A large sample plug prepared in a low-conductivity phosphate buffer (50 mM NaH2PO4, pH 2.5) was then hydrodynamically injected (5 psi, 80 s) into the capillary. Under an applied voltage of −30 kV, the analyte was accumulated at the FESS boundary and swept by the negatively charged micelles toward the UV detector. Plasma samples were pretreated by solid-phase extraction (SPE) to eliminate endogenous interferences. The validation results demonstrated a high coefficient of determination (r2> 0.9995) for the regression curve with impressive precision and accuracy: relative standard deviation (RSD) <5.86% and relative error <4.63%. The limit of detection (LOD, S/N = 3) for doripenem was determined to be 0.4 μg/mL. Compared to the conventional micellar electrokinetic chromatography method, our developed method achieved a sensitivity enhancement of up to 488-fold for doripenem. Furthermore, the newly developed method successfully quantified doripenem concentrations in plasma samples obtained from patients accepting doripenem regimens, proving its application potential in the clinical realm.Keywords:carbapenems;doripenem;FESS-sweeping MEKC;human plasma;online preconcentration
研究领域:
分析化学
·
临床医学
·
药理学
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2024
·Vol. 47
·期 21
·e70013
·
IF 2.8
Zhilei Li,Gangyuan Lin,Xiujuan Yang
A novel and rapid method was developed for the determination of galantamine in human plasma by microchip electrophoresis with a highly integrated contactless conductivity detector (CCD). The instrumental parameters affecting the response of the detector, such as excitation frequency and excitation voltage, were examined and optimized. The electrophoresis conditions that influenced the separation and detection of galantamine, including the composition of buffer solution, buffer pH, buffer concentration, additives, injection time, and separation voltage were systematically investigated. Under the optimal conditions, the peak height had a good linear relationship with the concentration of galantamine in human plasma from 10 to 160 µg/L, and the correlation coefficient was 0.9992, the limit of detection reached 1.1 µg/L. The recoveries were between 98.6% and 102.1%. This sensitive, rapid, and convenient method is a good alternative to existing methods for galantamine determination. Also, this highly integrated CCD holds great promise in clinical biochemical analysis.
研究领域:
分析化学
·
临床医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Journal of Pharmaceutical Analysis
·
2012
·
IF 0
Xiao-Hua Zhang,Hai-Long Wu,Jian-Yao Wang,Yao Chen,Yong-Jie Yu,Chong-Chong Nie,Chao Kang,De-Zhu Tu,Ru-Qin Yu
The effectiveness of traditional Chinese medicine (TCM) against various diseases urges more low cost, speed and sensitive analytical methods for investigating the phamacology of TCM and providing a theoretical basis for clinical use. The potential of second-order calibration method was validated for the quantification of two effective ingredients of Schisandra chinensis in human plasma using spectrofluorimetry. The results obtained in the present study demonstrate the advantages of this strategy for multi-target determination in complex matrices. Although the spectra of the analytes are similar and a large number of interferences also exist, second-order calibration method could predict the accurate concentrations together with reasonable resolution of spectral profiles for analytes of interest owing to its ‘second-order advantage’. Moreover, the method presented in this work allows one to simply experimental procedure as well as reduces the use of harmful chemical solvents.
研究领域:
中药学
·
分析化学
✓ 已验证
DOI
PubMed
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.
研究领域:
药理学
·
临床医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2019
·
IF 2.813
Tengfei Li,Bin Huang,Duo Li,Yantong Zhu,Li Ding,Chang Shu
In this work, we developed and validated the specific, sensitive and simple LC–MS/MS method for quantification of eslicarbazepine in human plasma. The analyte samples were prepared through a simple one-step protein precipitation method by acetonitrile . The chromatographic separation was operated on an economical Hanbon ODS-2 C18 column (150 mm × 2.1 mm, 10 μm) with isocratic elution using 10 mM ammonium acetate containing 0.01% formic acid and acetonitrile (72:28, v/v) as the mobile phase at the flow rate of 0.5 mL/min. The mass quantification was carried on the multiple reaction monitoring (MRM) of the transitions of m / z 255.1 → 194.1 for eslicarbazepine and m / z 446.1 → 321.1 for glipizide (the internal standard), respectively. The established method was validated with acceptable specificity, linearity, accuracy, precision, extraction recovery, matrix effect and stability in accordance with FDA regulations. At last, the validated method was successfully applied to determination of eslicarbazepine in human plasma obtained from clinical study.
研究领域:
药物分析
·
临床药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2016
·
IF 4.035
Jing Chen,Bao Qiong Li,Min Li Xu,Xue Wang,Yu Hong Jing,Hong Lin Zhai
The interference signals and overlapped peaks are common phenomena in fluorescence determination, which seriously influence the accuracy and reliability of analytical results. In this paper, Krawtchouk image moment method was introduced to the analysis of fluorescence three-dimensional (3D) spectra and applied to the quantitative analysis of three drugs including nicotinic acid, metoprolol and amlodipine in human plasma. Without any pretreatment to the obtained spectra, Krawtchouk moments were directly calculated on the grayscale images of 3D spectra, and the quantitative linear models for the three drugs were established by stepwise regression, respectively. The determination coefficients ( R ) were more than 0.9906. The correlation coefficients of leave-one-out cross-validation ( R cv ) were more than 0.9256. The precisions (RSD, %) of inter-day and intra-day variations were less than 8.4% and 3.1%, separately. The recovery was from 101.84% to 107.88%. The limit of quantification and the limit of detection were 0.12 μg mL −1 and 0.43 μg mL −1 , respectively. All the statistical parameters supported that the obtained models performed well and the proposed method was accurate and reliable. Our study indicates that Krawtchouk image moments with the powerful abilities of multi-resolution and extracting local information can be applied to the simultaneous determination of multi-target compounds in plasma based on fluorescence 3D spectra.
研究领域:
分析化学
·
药理学
·
医学检测
✓ 已验证
产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2013
·Vol. 28
·期 7
·994-1002
·
IF 1.945
Ting Zhou,Ting Zhao,Qing Cheng,Shan Liu,Ling Xu,Wen Tan
A sensitive liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of R -bambuterol and its active metabolite R -terbutaline in human plasma and urine was established. The inhibition for the biotransformation of R -bambuterol in plasma was fully investigated. Plasma samples were prepared on ice and neostigmine metilsulfate added as a cholinesterase inhibitor immediately after sample collection. All samples were extracted with ethyl acetate and separated on a C 18 column under gradient elution with a mobile phase consisting of methanol and water containing 5 m m ammonium acetate at a flow rate of 0.6 mL/min. The analytes were detected by an API 4000 tandem mass spectrometer with positive electrospray ionization in multiple reaction monitoring mode. The established method was highly sensitive with the lower limit of quantification (LLOQ) of 10.00 pg/mL for each analyte in plasma. In urine samples, the LLOQs were 20.00 and 500.0 pg/mL for R -bambuterol and R -terbutaline, respectively. The intra- and inter-day precisions were <12.7 and <8.6% for plasma and urine, respectively. The analytical runtime within 6.0 min per sample made this method suitable for high-throughput determination. The validated method has been successfully applied to the human pharmacokinetic study of R -bambuterol involving 10 healthy volunteers. Copyright © 2013 John Wiley & Sons, Ltd.
研究领域:
药理学
·
分析化学
·
临床医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
SEPARATION AND PURIFICATION TECHNOLOGY
·
2022
·
IF 9.136
Rui Chen,Xianzhao Zhang,Fengmao Liu,Chengcheng Liu,Qingrong Peng,Xiaoqiang Qiao
Conductor-like screening model for realistic solvents (COSMO-RS) theoretical chemical model is an effective tool for predicting the thermodynamic properties of solvents. In this study, 144 ionic liquids (ILs) were designed and screened by COSMO-RS with affinity interactions with benzimidazoles (BZDs) as the target. Ionic liquid-based magnetic nanoparticles (IL-MNPs, Fe 3 O 4 @SiO 2 @MAPs@PIL-POSS) were prepared by the selected diene ILs (1-allyl-3-vinylimidazolium chloride [Avim]Cl) and polyhedral oligomeric silsesquioxane (POSS) coating Fe 3 O 4 by free radical polymerization. As the adsorbent, the Fe 3 O 4 @SiO 2 @MAPs@PIL-POSS has great magnetic recovery ability and excellent specific adsorption ability for BZDs. The magnetic dispersive solid-phase extraction (MDSPE) of BZDs was established by optimizing the adsorption and desorption parameters. It is worth noting that the sample pretreatment only took 5 min. Combined with HPLC-MS/MS, a trace detection method for 7 trace BZDs in human plasma was established. In the method validation, the recoveries ranged from 79 % to 99 %, with relative standard deviations (RSDs) of 1.8 % to 8.8 %. The linear range were 1–1,000 μg/L. As a representative BZD, the adsorption kinetics and thermodynamic behavior of carbendazim on Fe 3 O 4 @SiO 2 @MAPs@PIL-POSS were analyzed to verify the adsorption mechanism, which is consistent with the results of IL screened by COSMO-RS. Therefore, it is feasible to theoretically screen IL and design IL-MNPs as specific adsorption materials. Furthermore, the theoretical design of MDSPE methods for target molecules has potential.
研究领域:
分析化学
·
药物分析
·
材料科学
✓ 已验证
产品关联
DOI
高影响因子
Toxics
·
2025
·Vol. 13
·期 5
·352
·
IF 4.1
Yubing Yan,Bowen Liang,Jiawen Yang,Qing Deng,Xiaoying Liang,Hui Chen,Bibai Du,Lixi Zeng
Fluorescent brighteners (FBs) are a class of chemicals extensively used in industrial and consumer products. Their environmental occurrences and potential health risks have raised significant concerns. However, the lack of analytical methods for FBs in human samples has hindered the accurate assessment of internal exposure levels. Addressing this gap, this study developed and validated a novel method for the simultaneous determination of 13 FBs at trace levels in human plasma using solid-phase extraction combined with HPLC-MS/MS. The method employed EMR-Lipid SPE columns, which can selectively adsorb phospholipids for plasma sample pre-treatment. Detection was achieved through positive ion electrospray ionization (ESI) in multiple reaction monitoring (MRM) modes. The results showed that all 13 FBs exhibited good linearity within their respective ranges, with correlation coefficients (R2) greater than 0.992. The method quantitation limits (MQLs) of the FBs ranged from 0.012 to 0.348 ng/mL, and the spiked recovery rates ranged from 61% to 98%. The method was successfully applied to analyze 10 adult plasma samples, detecting 10 FBs with total concentrations ranging from 0.221 to 0.684 ng/mL. This study provides a reliable analytical method for determining FBs in human plasma, providing a basis for further research on human internal exposure to FBs and associated health risk assessments.
研究领域:
分析化学
·
环境健康学
·
毒理学
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2022
·Vol. 45
·期 10
·1818-1826
·
IF 3.614
Yinghao Wang,Xianxie Zhang,Wenya Hu,Chenglong Dong,Dali Fu,Sara Girmay Habtegabir,Yehua Han
Free fatty acids are involved in many metabolic regulations in the human body. In this work, an ultra-fast screening method was developed for the analysis of free fatty acids using trapped ion mobility spectrometry coupled with mass spectrometry. Thirty-three free fatty acids possessing different unsaturation degrees and different carbon chain lengths were baseline separated and characterized within milliseconds. Saturated, monounsaturated, and polyunsaturated free fatty acids showed different linearities between collision cross-section values and m/z . The establishment of correlations between structures and collision cross-section values provided additional qualitative information and made it possible to determine free fatty acids which were out of the standards pool but possessed the confirmed linearity. The gas-phase separation made the quantitative analysis reliable and repeatable at a much lower time cost than chromatographic methods. The sensitivity was comparable to and even better than the reported results. The method was validated and applied to profiling free fatty acids in human plasma. Saturated free fatty acids abundance in the fasting state was found to be lower than that in the postprandial state, while unsaturated species abundance was found higher. The method was fast and robust with minimum sample pretreatment, so it was promising in the high-throughput screening of free fatty acids.
研究领域:
分析化学
·
代谢组学
·
医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Current Pharmaceutical Analysis
·
2022
·Vol. 18
·期 10
·919-929
·
IF 0.743
Gao Pan,Zou Qiao-gen
Background: Perampanel (PER) is a third-generation antiepileptic drug (AED). Several methods have been developed for the quantification of perampanel in plasma. The pharmacokinetic characteristics of perampanel in healthy Chinese ubjects have not been comprehensively reported.
Objective: A simple, fast and sensitive LC-MS/MS method was established and validated for the quantification of perampanel in human plasma and its application to a bioequivalence study. Methods: Chromatographic separation was accomplished on a ZORBAX Eclipse XDB-Phenyl column (4.6 mm
× 75 mm, 3.5 μm) using a binary gradient with mobile phase (A) (water containing 5 mmol/L ammonium acetate and 0.1% formic acid and (B) acetonitrile-water (95:5, v/v) at a flow rate of 0.9 mL/min and sample preparation was by one-step protein precipitation via acetonitrile. Results:
The total run time in this study was 4.5 min and the retention time of perampanel and perampanel-d5 (internal standard) were 2.30 min and 2.32 min, respectively. The method was developed and validated over the concentration range of 2.00-500 ng/mL for perampanel, with a correlation coefficient
greater than 0.9992. The inter-day precision was 3.1%-3.8% and accuracy was 98.9%-103.5%. The intra-day precision was 2.4%-6.8% and the accuracy was 97.6%- 104.9%. The extraction recovery ranged from 99.23%-103.84% and the matrix effect was not significant. Perampanel was proved to be stable
in solution and human plasma under different tested conditions. The validated method was successfully applied to a randomized, open-label, 2- period, crossover bioequivalence study in healthy Chinese subjects, and the results indicated that bioequivalence was achieved for 2 formulations of
the 4-mg perampanel tablet under both fasting and fed conditions, and both treatments were safe and well-tolerated by all study subjects. Conclusion: The validated method was successfully applied to a bioequivalence study of perampanel in human plasma and has achieved satisfactory results.
研究领域:
药理学
·
分析化学
·
临床医学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）