JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2025
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IF 3.1
Lili Liu,Yaping Huang,Qingqing Wang,Ziyuan Wang,Ke Pan,Jian Zhang,Ying Peng,Guangji Wang,Zhiqi Yin,Jianguo Sun
As a plant with a rich history of medicinal and dietary use, Gynostemma pentaphyllum (Thunb.) Makino is predominantly characterized by the gypenosides. Contemporary research has demonstrated that these saponins possess significant hypolipidemic and hypoglycemic effects. This study focused on developing an LC-MS/MS approach to elucidate the pharmacokinetic profiles of 13 gypenosides in rat models. The separation was accomplished using a ZORBAX Eclipse Plus C18 column (2.1 mm × 100 mm, 1.8 µm). Detection was facilitated by employing positive electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The analytical method was fully validated, including selectivity, linear response, measurement precision, analytical accuracy, extraction efficiency, matrix interference, and sample stability. The lower limit of quantification (LLOQ) for all compounds was 10 ng/mL, with each exhibiting a favorable linear relationship (r ≥ 0.9960). The precision, as measured by the relative standard deviation (RSD) for intra-day and inter-day variability, did not exceed 8.41 %. The accuracy, expressed as the relative error (RE), varied from −4.42–8.42 %. The recovery rate of the extraction process was between 92.02 % and 114.77 %, and no notable matrix effects were detected. The stability of the compounds was confirmed under four distinct storage conditions. Pharmacokinetic results indicated that all analytes displayed rapid absorption, prolonged retention, and slow elimination in rats, and exhibited nonlinear pharmacokinetics at low, medium, and high dosage levels. This study has established a quantification method for 13 gypenosides and successfully applied it to their pharmacokinetic studies in rats, providing a foundation for their further development and utilization.
研究领域:
中药学
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分析化学
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药理学
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Horticulturae
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2025
·Vol. 11
·期 12
·1417
·
IF 3
Mingzheng Duan,Liuyuan Bao,Ting Jiang,Kangjian Song,Yubo Chen,Sijiu He,Xiande Duan,Muhammad Ikram,Shunqiang Yang,Muhammad Junaid Rao
Strawberry fruit quality is linked to its phytochemical composition, yet the diversity of non-volatile terpenoids remains largely unexplored. Therefore, a comparative LC-MS/MS-based metabolomic analysis of terpenoid profiles was conducted using three commercial cultivars (Fragaria×ananassa) and a wild accession ofFragaria nilgerrensis(HM). Results from this study showed that the HM cultivar had a total terpenoid abundance 5–6 times higher than the commercial cultivars. The HM cultivar was uniquely enriched in specific triterpenoids, such as 3β,6β,19α,24-Tetrahydroxyurs-12-en-28-oic acid and 13,27-Cyclo-2,3-Dihydroxy-11,19(29)-Ursadien-28-Oic Acid, which was over 450 times higher than the ‘Danxue’ and ‘Fenyu’ commercial strawberry cultivars. Conversely, sesquiterpenoids like Alismol and Pterocarpol were 100 times lower in HM than in the commercial cultivars. This enhanced triterpenoid accumulation strongly correlated with a superior capacity to scavenge free radicals in vitro, with HM showing maximum capacity, as measured by the DPPH assay. These findings highlight the value of wild strawberry germplasm as a reservoir of biochemical diversity for breeding strawberries with enhanced functional quality.
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MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Ziyuan Zheng,Wenguang Yan,Wenlong Liu,Zihao Cai,Yanjun Ding,Jiang Ling
Volatile organic compounds (VOCs) play a critical role in human physiology, with their concentrations serving as key indicators of physiological states. Among these, trans-4,5-epoxy-(E)-2-decenal, a volatile organic compound found in mammalian blood, exhibits unique chemical reactivity and olfactory sensitivity due to its molecular structure, which is closely associated with lipid peroxidation processes. However, conventional detection methods, such as gas chromatography-olfactometry-mass spectrometry (GC-O-MS), suffer from limitations including inherent subjectivity, poor reproducibility, stringent operational requirements, and low throughput, which undermine their clinical reliability. To address these challenges, this study developed an optimized liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for accurate qualitative and quantitative analysis. Given the poor detectability of aldehydes via LC-MS/MS, 2,4-dinitrophenylhydrazine (DNPH) derivatization was employed to enhance the chromatographic behavior and retention of the target compound. Additionally, HLB solid-phase extraction (SPE) columns was employed for purification to enhance the sensitivity of LC-MS/MS for the detection of trans-4,5-epoxy-(E)-2-decenal. Following derivatization, trans-4,5-epoxy-(E)-2-decenal demonstrated strong retention during chromatographic separation. The mobile phase, composed of acetonitrile and ultrapure water, exhibited significantly superior performance compared to combinations of acetonitrile with ammonium acetate buffer. Under optimized conditions, the LC-MS/MS method demonstrated excellent linearity for trans-4,5-epoxy-(E)-2-decenal within a range of 1–300 ng/mL, with correlation coefficient (R 2 ) of 0.9984, detection limit (LOD) of 0.3 ng/mL. The relative standard deviation (RSD) for spiked blood samples in the experiment was 12.53 %.
研究领域:
分析化学
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生物化学
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医学诊断
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代谢组学
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质谱分析
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Journal of Environmental Sciences
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2024
·
IF 5.9
Shuang Chen,Yue Qiao,Youwei Jiang,Wei Qiu,Shuang Zang,Jing Zhang,Xianshi Wang,Jun Ma
Halogenated aromatic disinfection byproducts (DBPs) are gradually receiving attention due to their high detection frequency and usually higher toxicity than regulated DBPs. In this study, we established a solid phase extraction (SPE)-LC-MS/MS method to simultaneously trace analyze 59 halogenated aromatic DBPs. The limits of detection and limits of quantification of halogenated aromatic DBPs ranged from 0.03 ng/L to 135.23 ng/L and 0.1 ng/L to 450.76 ng/L, respectively. The range of recoveries and relative standard deviation (RSD) in river water were between 72.41 % to 119.54 % and 1.86 % to 16.03 %, respectively. Therefore, this method can be used to accurately analyze trace levels of halogenated aromatic DBPs in drinking water. The occurrence and transformation of halogenated aromatic DBPs were explored based on this method. In the chlorinated simulated source water and chlorinated river water, 20 and 45 halogenated aromatic DBPs were determined, respectively. The active halogen species (HOCl, HOBr, and HOI) first reacted with natural organic matter (NOM) to form halogenated aromatic DBPs. Then, chlorine further reacted with the halogenated aromatic DBPs to convert them into small-molecule halogenated aliphatic DBPs through oxidation, electrophilic substitution, and hydrolysis reaction, etc. In the chlorinated simulated source water, chlorinated river water, and tap water, the toxicity contribution of bromoacetic acids (Br-HAAs) accounted for the majority (> 71.16 %). Given that halogenated aromatic DBPs are intermediate products of halogenated aliphatic DBPs, controlling the formation of halogenated aromatic DBPs is beneficial in decreasing the formation of halogenated aliphatic DBPs, thereby diminishing the toxicity of drinking water.
研究领域:
环境科学
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分析化学
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公共卫生
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高影响因子
MICROCHEMICAL JOURNAL
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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.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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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.
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BIOMEDICAL CHROMATOGRAPHY
·
2023
·Vol. 37
·期 12
·e5751
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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.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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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.
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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.
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BIOMEDICAL CHROMATOGRAPHY
·
2018
·Vol. 32
·期 6
·e4192
·
IF 1.688
Dan Li,Gang Zhao,Weipeng Ai,Gao Li,Luqin Si,Jiangeng Huang,Yunzhou Chen,Sanlan Wu
In this study, a liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated to simultaneously determine the anticancer drugs etoposide and paclitaxel in mouse plasma and tissues including liver, kidney, lung, heart, spleen and brain. The analytes were extracted from the matrices of interest by liquid–liquid extraction using methyl tert -butyl ether–dichloromethane (1:1, v/v). Chromatographic separation was achieved on an Ultimate XB-C 18 column (100 × 2.1 mm, 3 μm) at 40°C and the total run time was 4 min under a gradient elution. Ionization was conducted using electrospray ionization in the positive mode. Stable isotope etoposide-d3 and docetaxel were used as the internal standards. The lower limit of quantitation (LLOQ) of etoposide was 1 ng/g tissue for all tissues and 0.5 ng/mL for plasma. The LLOQ of paclitaxel was 0.4 ng/g tissue and 0.2 ng/mL for all tissues and plasma, respectively. The coefficients of correlation for all of the analytes in the tissues and plasma were >0.99. Both intra- and inter-day accuracy and precision were satisfactory. This method was successfully applied to measure plasma and tissue drug concentrations in mice treated with etoposide and paclitaxel-loaded self-microemulsifying drug-delivery systems.
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2018
·
IF 2.441
Qiong Lou,Jun Wen,Yuanying Jiang,Jinghua Huang,Guorong Fan,Fenyun Song
A reliable liquid chromatography/tandem mass (LC-MS/MS) method was developed for quantitation of 3′, 4′-dimethoxy flavonol-3-β- d -glucopyranoside (DF3G) in rat plasma using pantoprazole as the internal standard. An Agilent C18 column (100 mm × 3 mm, 3.5 μm) was performed for chromatographic separation with the mobile phase composed of methanol-water (containing formic acid) at a flow rate of 0.4 mL/min. A triple-quadrupole mass spectrometry equipped with an electrospray ionization (ESI) source in positive ion mode was applied to quantitative analysis by multiple reacting monitoring (MRM). The MRM precursor-product ion transition of DF3G and Pantoprazole (IS) were m / z 461.1 → 299.2 and 383.9 → 200.2, respectively. Calibration curves were recovered in a concentration range of 1–500 ng/mL for plasma with a limit of lower quantification (LLOQ) of 1 ng/mL. The intra-day and inter-day precision were not >10%. The accuracy of DF3G ranged from −10% to 0.53% in quality control (QC) samples at three concentrations. DF3G was not degraded during the analysis and the storage period. All the data were validated in accordance with the FDA bioanalytical method validation guideline. The LC-MS/MS method was successfully employed in the pharmacokinetic study of the DF3G after oral administration and intravenous injection in rats.
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JOURNAL OF FOOD AND DRUG ANALYSIS
·
2018
·
IF 2.852
Xiujuan Chen,Chen Liang,Lijun Cui,Jian Le,Zheyuan Qian,Runsheng Zhang,Zhanying Hong,Yifeng Chai
Combinations of new antidepressants like duloxetine and second-generation antipsychotics like quetiapine are used in clinical treatment of major depressive disorder, as well as in forensic toxicology scenarios. The drug–drug interaction (DDI) between quetiapine and duloxetine is worthy of attention to avoid unnecessary adverse effects. However, no pharmacokinetic DDI studies of quetiapine and duloxetine have been reported. In the present study, a rapid and sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for simultaneous determination of quetiapine and duloxetine in rat plasma. A one-step protein precipitation with acetonitrile was applied for sample preparation. The analytes were eluted on an Eclipse XDB-C 18 column using the mixture of acetonitrile and 2 mM ammonium formate containing 0.1% formic acid at a gradient elution within 6.0 min. Quantification was performed in multiple-reaction-monitoring mode with the ion transitions m/z 384.4 → 253.2 for quetiapine, m/z 298.1 → 154.1 for duloxetine and m/z 376.2 → 165.2 for IS (haloperidol), respectively. Good linearity was obtained in the range of 0.50–100 ng/mL for quetiapine (r 2 = 0.9972) and 1.00–200 ng/mL for duloxetine (r 2 = 0.9982) using 50 μL of rat plasma, respectively. The method was fully validated with accuracy, precision, matrix effects, recovery and stability. The validated data have met the acceptance criteria in FDA guideline. The method was applied to a pharmacokinetic interaction study and the results indicated that quetiapine had significant effect on the enhanced plasma exposure of duloxetine in rats under combination use. This study could be readily applied in therapeutic drug monitoring of major depressive disorder patients receiving such drug combinations.
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