ANALYTICA CHIMICA ACTA
·
2021
·
IF 6.558
Qianqian Shang,Hang Mei,Xinrui Feng,Chuixiu Huang,Stig Pedersen-Bjergaard,Xiantao Shen
Electromembrane extraction (EME), involving the migration of charged analytes across a supported liquid membrane (SLM) with an external power supply, is a promising sample preparation method in analytical chemistry . However, the presence of boundary double layers at the SLM/solution interfaces often restricts extraction efficiency. To avoid this, the current work proposed an ultrasound-assisted EME (UA-EME) method based on a novel type of supported semi-liquid membrane (SsLM). The characterizations showed that the SsLM was stable under ultrasound conditions. Ultrasound was found to reduce the boundary double layers and thus increase the mass transfer. Major operational parameters in UA-EME including ultrasound power density, temperature, applied voltage and extraction time were optimized with haloperidol , fluoxetine , and sertraline as model analytes. Under the optimal conditions, extraction recoveries of model analytes in water samples were in the range of 66.8%–91.6%. When this UA-EME method was coupled with LC-MS/MS for detection of the target analytes in human urine samples, the linear range of the analytical method was 10–1000 ng mL −1 , with R 2 > 0.997 for all analytes. The limits of detection (LOD) and limits of quantification (LOQ) were in the range of 1.7–2.1 ng mL −1 and 5.7–6.7 ng mL −1 , respectively. The UA-EME expands the application field of ultrasound chemistry and will be very important in development of stable and fast sample preparation systems in the future.
研究领域:
分析化学
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超声化学
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药物分析
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2022
·Vol. 61
·期 2
·130-139
·
IF 1.555
Sun Lu-Ning,Shen Ye,Yang Yu-Qing,Chen Xiang-Long,Huang Feng-Ru,Wang Dun-Jian,Zhang Ye,Wang Da-Wei,Wang Yong-Qing
The feasibility of taking the ratio of 6β-hydroxycortisol (6β-OHCOR) to cortisol (COR) in plasma as a biomarker to reflect CYP3A4 activity needs to be verified, but the low concentration of 6β-OHCOR which is an endogenous substance in plasma presents a challenge for determination. In this study, a Liquid chromatography with tandem mass spectrometry (LC–MS/MS) method was established to simultaneously quantify the COR and 6β-OHCOR in plasma with COR-d4 and 6β-OHCOR-d4 as internal standards (ISs). Plasma samples were treated by protein precipitation using acetonitrile. Separation with a gradient elution within 5 min was achieved on C18+ column utilizing 5 mM ammonium formate and methanol. An API 4,000 MS in multiple reaction monitoring mode with transitions of 407.1 → 361.1 and 423.1 → 347.1 was utilized. Albumin solution was used as a surrogate matrix, with good linearities over the concentration of 1.20–300 ng/mL for COR and 0.0400–10.0 ng/mL for 6β-OHCOR. The precisions for intrarun and interrun were < 6.8%, and the accuracy was fell in the interval of −5.2 to 3.5%. Matrix effect was not found. Recovery was close to 100.0%. Stability was confirmed under the storage and processing conditions. The validated method was applied to evaluate the inhibitory effect of voriconazole to CYP3A by the ratio of 6β-OHCOR to COR.
研究领域:
分析化学
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药理学
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临床医学
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产品关联
DOI
PubMed
高影响因子
BIOCHIMICA ET BIOPHYSICA ACTA-GENERAL SUBJECTS
·
2022
·
IF 4.117
Tan Qin,Yu Wang,Jing Nie,Lushan Yu,Su Zeng
Background Sodium taurocholate co -transportering polypeptide (NTCP, SLC10A1 ) is a vital bile acid transporter and the functional receptor of hepatitis B and D virus. The oligomerization of NTCP is important for the structural study of its interaction with HBV preS1 peptide. Methods Recombinant NTCPs were expressed in Sf9 host cell using baculoviruses. Function of recombinant NTCP was verified by liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) method. A quantitative fluorescence resonance energy transfer (FRET) method was established to analyze the interaction between NTCP wild type (WT) and mutants. Co-immunoprecipitation (Co-IP) was used to test the interaction between NTCP variants. Results Sub-cellular location of recombinant NTCPs varies with the modification of NTCP. Bands of monomer, dimer and oligomers were shown in gel analysis of NTCP. Significant FRET was observed between cyan florescence protein (CFP) tagged NTCP and yellow florescence protein (YFP) tagged NTCP. FRET efficiency between CFP- and YFP-NTCP S267F mutants was lower than WT. Co-IP results showed that S267F interacts with WT NTCP when co-expressed in cell. Conclusion Dimer is the predominant form of NTCP expressed in Sf9 when solubilized with detergent. FRET and Co-IP analysis support that NTCP forms oligomers in Sf9 cell. General significance Our results showed that NTCP formed oligomers in Sf9 cell. Meanwhile the FRET analysis of NTCP variants further elucidated the molecular mechanism of NTCP oligomerization.
研究领域:
病毒学
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分子生物学
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细胞生物学
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2018
·
IF 2.831
Mengzhe Guo,Dantong Liu,Qian Sha,Houfa Geng,Jun Liang,Daoquan Tang
The epigenetic modification of DNA or RNA may have relationship with the development of diabetic nephropathy (DN). We designed to develop a liquid chromatography mass spectrometry (LC–MS) coupled with mobile phase additive sensitization method for the analysis of the dissociative epigenetic modified nucleosides in serum of patients from different periods of DN with the health comparison. Serum samples were collected from 43 healthy volunteers and 156 patients, which divided into four groups. A succinic acid enhanced LC–MS/MS strategy was developed for the quantitative analysis of seven nucleosides in serum samples. The signal intensity of seven nucleosides increased three to seven times, respectively. A series of statistical analysis were carried out to demonstrate the dynamic changes of modified nucleosides in four groups. This method showed good specific, accuracy, and stability. The results were calibrated and presented through the formation of m 6 A/C, I/C, 5-mdC/C, 5-mC/C, pseU/U to eliminate the individual and age differences. The m 6 A/C, I/C, and pseU/U were found having the dynamic changes in four groups ( p < 0.05). And these five modified nucleosides can also used as one parameter to distinguish these four groups by ROC and LDA analysis. Additionally, they were found to be connected with several clinical biochemical indexes through multiple linear regression analysis. Our LC–MS/MS method assay successfully quantifies the modified nucleosides in serum. And three modified nucleosides can act as the potential biomarkers to describe the development of DN and help to evaluate the diagnosis, treatment, and prognosis of DN in clinical.
研究领域:
医学
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分子生物学
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分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2018
·
IF 2.831
Teng-Fei Yuan,Juan Le,Yan Cui,Rui Peng,Shao-Ting Wang,Yan Li
Background Comprehensive serum sex hormone profiling is essential for monitoring the occurrence and development of many related diseases. However, the current methods for multi-class sex hormone detection were always lack of Standard Reference Material (SRM) certification and suffered from large sample consumption. For improvement, we developed a new liquid chromatography-tandem mass spectrometry (LC–MS/MS) method focused on SRM certification and minimization of serum consumption for simultaneous quantification of seven mainstream serum sex hormones including estrogens (estrone E1, estradiol E2 and estriol E3), androgens (testosterone T, androstenedione AD, dehydroepiandrosterone DHEA) and progestogens (progesterone P). Methods To achieve one-batch analysis, a straightforward strategy was designed and carefully optimized. Schematically, serum was firstly spiked with isotope-labeled internal standards. Then, liquid-liquid extraction was performed with methyl tert-butyl ether. After drying under nitrogen, dansyl chloride was introduced for derivatization. Finally, the mixture was submitted to LC–MS/MS for quantification. Results The limit of quantification was 0.005 ng/mL for E1, E2 and E3, 0.01 ng/mL for T, P and AD, 0.25 ng/mL for DHEA. Inter- and intra-assay CVs were less than 11.8%. The selectivity was proved satisfactory by interference spiking tests. With systematical SRM validation, the mean bias of −5.4 to 4.7% was observed, which indicated excellent method reliability. We found significant positive bias in chemiluminescence immunoassay (CLIA) detection comparing with current method, which promoted us to reconsider our previous results on sex hormone regulation in male patients with coronary atherosclerotic disease. After redetecting the related samples, modified and improved conclusions were proposed. Conclusions A LC–MS/MS method for multi-class serum sex hormone profiling was developed with SRM certification and minimized serum consumption. Taking advantages of such reliable method, the previous CLIA-based research findings on sex hormone regulation in male patients with coronary atherosclerosis were modified and improved after redetecting the same sample-pool.
研究领域:
医学检验
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内分泌学
·
临床化学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 3
·e6090
·
IF 1.7
Fang Wang,Wenfei Sun,Zheheng Ma,Furui Chu
Proteolysis targeting chimera (PROTAC) has been developed and currently enjoys widespread interest among the field of pharmaceutical manufacturing in recent decades. NX-5948 is an orally active PROTAC Bruton tyrosine kinase degrader, which shows anti-inflammatory and antitumor activities. In this study, a simple and fast bioanalytical method for the quantification of NX-5948 in beagle dog plasma was developed using liquid chromatography–tandem mass spectrometry (LC-MS/MS). A full method validation was performed according to regulatory guidelines. For the quantification, [M + H] + was formed using an electrospray ionization (ESI) source in the positive ion mode, and selective reaction monitoring (SRM) was employed using a triple quadrupole mass spectrometry. The monitored precursor-to-product transitions were m/z 807.5 > 790.5 for NX-5948 and m/z 812.4 > 452.1 for internal standard. A linear response was obtained at the concentration range of 0.5–200 ng/mL, with correlation coefficient > 0.99. The interday accuracy ranged from −9.03% to 5.99% (RSD < 7.84%), and the intraday accuracy from −5.15% to 8.56% (RSD < 6.90%). NX-5948 was demonstrated to be stable under the present storage conditions. After validation, the method was successfully applied for the quantification of NX-5948 in beagle dog plasma after oral and intravenous administration of the NX-5948.
研究领域:
药物分析
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生物制药
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临床药理学
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产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2018
·Vol. 23
·期 3
·543
·
IF 3.098
Zhi-Feng Li,Meng-Ying Zhou,Ting Tan,Chen-Cong Zhong,Qi Wang,Shi-Lin Yang,Yu-Lin Feng,Hui Ouyang
Ziyuglycoside I (ZGS1) is a promising drug candidate for the treatment of leucopenia. Currently, information on ZGS1 and its in vivo metabolite ziyuglycoside II (ZGS2) is limited. The objective of this study was to investigate the pharmacokinetics, tissue distribution, and excretion of ziyuglycoside I (ZGS1) and its metabolite ziyuglycoside II (ZGS2) in rats. In our study, a simple and sensitive high-performance liquid chromatography-mass spectrometry (HPLC-MS/MS) method was established for simultaneous determination of ZGS1 and its metabolite for Sprague-Dawley rat pharmacokinetics studies. The method was validated following internationally-approved guidelines. The results presented in this study indicated that subcutaneous administration of ZGS1 prolonged its extension time and increased the area under the curve (AUC0–t) of ZGS2 during 0 to t minutes. In summary, in this study, the pharmacokinetic characteristics of ZGS1 and its metabolite ZGS2 were defined and its tissue distribution, and excretion in rats were described. Our finding may be beneficial for leucopenia drug that focus on ZGS1.Keywords:ziyuglycoside I (ZGS1);ziyuglycoside II (ZGS2);LC-MS/MS;pharmacokinetics;tissue distribution;excretion
研究领域:
药物代谢
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药理学
·
分析化学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2023
·
IF 3
Xin Wei,Liang Cao,Mingrui Zhou,Jiana Huang,Xiaoyan Liang,Nijie Li,Yanan Pan,Renli Yin,Huashou Li,Adela Jing Li
Emerging pesticides of neonicotinoids (NEOs) and “Universal Pesticides” (UPs) are a growing global concern due to their growing commercial importance and potential risks to human health. The currently available analytical methods for these pesticides in biomonitoring were usually tailored for limited number of analytes, or were time consuming and costly. In this study, an efficient and sensitive method for the analysis of 16 NEOs and nine UPs in human follicular fluid (FF) was developed by using a salting-out assisted liquid-liquid extraction (SALLE) method and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Method performance was evaluated by calibration linearity ( r > 0.99), sensitivity at limits of quantification (0.01–0.50 ng/mL), accuracy at relative recoveries (81–117%) and precision at relative standard deviations (≤16%). The developed method was further validated by analyzing 21 human FF samples that were collected from a hospital in Guangzhou, China. Among the 25 study analytes, two NEOs and six UPs had their detection rates over 85% and medians at 0.048–0.808 ng/mL in the FF samples. Considering the well-known toxicity of these pesticides and their metabolites, it is urgent to figure out exposure profiles of study pesticides and potential reproductive risk for women. To the best of our knowledge, this study is the first to develop and apply the SALLE method in the extraction of 16 NEOs and nine UPs simultaneously in human FF.
研究领域:
环境科学
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分析化学
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生殖健康
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DOI
PubMed
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2016
·
IF 2.711
Xiaoqun Wei,Linzhou Zhuang,Chaomin Wu,Wenrui Chen,Zhiyong Li,Baojun Xu
A novel method for quantitative analysis of ethylenediaminotetracetic acid (EDTA) in wines and beers by liquid chromatography coupled to tandem mass spectrometry has been developed. Positive-ion mode was applied as the scan mode, amine species were firstly used as the derivatization reagents of EDTA, and phenylboronic acid was used to react with maltose to eliminate its matrix interference. Primary amines could efficiently eliminate the interference from metal ions (Fe(III) and Cu(II)). The responsive intensity of EDTA with amine derivatization could be improved over 300 times than that without adding amine species. The recovery rate was significantly increased to 104.1% after adding phenylboronic acid at 20.0 mg/L as compared to the control spike-and-recovery experiment results (1.3–1.7%) of beer samples without adding phenylboronic acid. The validated method showed excellent detection sensitivity (0.001 mg/L for LOD (limit of detection) and 0.004 mg/L for LOQ (limit of quantification)) with satisfactory recovery rates (76.0%–97.2%), and good precision (1.40–5.40% RSD values). The optimized method has been satisfactorily applied to the analysis of actual wine and beer samples. It can be proposed as a powerful analytical method of EDTA in wines and beers, and can even be adapted to detect other chelates and polydentate compounds.
研究领域:
分析化学
·
食品科学
✓ 已验证
DOI
高影响因子
Scientific Reports
·
2026
·
IF 4.9
Zhu Lian,Liu Jin,Li Kailin,Wang Yang,Liu Fengjiao,Xie Liu,Zhang Yan,Cai Wei
Tryptophan is an essential amino acid for the human body, and its metabolic processes are closely related to a variety of physiological and pathological processes, including neurodegenerative diseases, immune modulation, and cardiovascular diseases. Simultaneous detection of tryptophan and its nine metabolites is challenging and previous methods may have shortcomings of poor sensitivity, selectivity, and specificity in complex matrices. The technology of LC-MS/MS, with its characteristics of high sensitivity and selective, provides a powerful tool for the detection of biomarkers. A rapid and effective method for the simultaneous determination of kynurenine metabolites (Xanthurenic acid (XA), DL-Tryptophan (TRP), Kynurenine (KYN), 3-Hydroxyanthranilic acid (3-HAA), Quinolinic acid (QUIA), Kynurenic acid (KYNA), 3-Hydroxy-DL-kynurenine (3HK), 2-Picolinic acid (2PA), 5-Hydroxytryptamine (5-HT), and Anthranilic acid (AA)) was established in human plasma using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) technology. Methanol precipitation was used for sample pretreatment, with [2H5]-L-Tryptophan (TRP-D5) as the internal standard. Mass spectrometric detection was performed in positive electrospray ionization mode using multiple reaction monitoring on a triple-quadrupole mass spectrometer. The method’s selectivity, linearity, quantification limit, detection limit, precision, recovery rate, matrix effect, and stability are evaluated. The results show that the linear ranges of 2PA, QUIA, 3HK, 5HT, KYN, 3HAA, TRP, XA, KYNA and AA are 0.25-50, 0.9–225, 1.2–120, 1.4–700, 2-2000, 0.15–150, 180-180000, 0.1–100, 0.1–100, and 0.2–100 ng/mL, respectively; all analytes have good linear relationships with a determination coefficient R2 greater than 0.99. The precision relative standard deviation (RSD) is less than 15%; the spiked recovery rate is 87.54%-107.43%, with an RSD of 2.76%-12.19%. Additionally, the matrix effects for 10 analytes are summarized. At all three QC levels, the matrix effect in plasma is 88.44% to 107.85%, and the RSD is 2.97%-14.62%. These results indicate that there is no significant matrix effect. Stability was evaluated by comparing the measured concentrations after storage with the initial concentrations and expressed as percentages of the initial values. All analytes remained within 85–115% of the initial concentrations under the tested conditions. This study describes the development and validation of a rapid, sensitive, and robust UHPLC–MS/MS method for the simultaneous quantification of ten kynurenine pathway metabolites—including the precursor tryptophan, key intermediates, and neurotoxic/neuroprotective end products-in human plasma. The method employs a simple protein precipitation procedure, a single deuterated internal standard (TRP-D5), and a 13-minute chromatographic run on a C8 column, providing adequate separation of metabolites with diverse physicochemical properties.
✓ 已验证
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2025
·
IF 6.7
Zhiye Yan,Weiwei Tang,Bin Li
Metabolomics is a potent tool used for discovering disease biomarkers and investigating intricate mechanisms of diseases by analyzing metabolite changes in biological systems. However, challenges in metabolite detection have not been fully addressed due to their vast physicochemical diversity and broad concentration range, impacting comprehensive profiling of the metabolome, particularly for certain metabolites with limited detection sensitivity. Therefore, a novel chemical derivatization method based on hydralazine (HZN) was developed for highly sensitive detection of various poorly ionized small metabolites in biological samples using liquid chromatography–tandem mass spectrometry (LC–MS/MS). HZN-based multifunctional derivatization mainly targeted metabolites with carbonyl, carboxyl, and phosphoryl groups, such as free fatty acids, keto-acids, hydroxy acids, bile acids, fatty aldehydes, and phosphoryl compounds. Main parameters affecting the derivatization efficiency were investigated, such as the condensation reagent, and optimal conditions were obtained. The labeling of HZN enabled the generation of characteristic fragment ions through collision-induced dissociation, avoiding the laboriousness of deducing MS/MS fragmentation and facilitating large-scale quantitative analysis. The sensitivities of HZN-derivatized metabolites improved significantly, ranging from 10 to 5000-fold, and the limits of quantitation for derivatized metabolites varied from 5 pM to 100 nM, depending on their structures. Furthermore, alterations of various gut microbiota-derived metabolites in mice fed with a high-fat diet were unraveled using the HZN-based derivatization method, indicating its promising applications in the investigation of disease-related changes in the metabolome.
研究领域:
代谢组学
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分析化学
·
质谱分析
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生物医学研究
·
分子生物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY
·
2021
·
IF 2.826
Xiangwu Liu,Bangyan Song,Xiaoxia Jiang,Ya Yang,Ping Lu,Deyu Hu
A quick, easy, cheap, effective, rugged and safe liquid chromatography-tandem mass spectrometry technology was used to determine benziothiazolinone in citrus. Orthogonal test and single-factor analysis were conducted to identify the optimal extraction method of benziothiazolinone. The good linearity (R2 > 0.9949), high accuracy and precision, matrix effect and satisfactory recoveries (79.31%–98.68%) at three spiked levels (0.02, 0.2 and 2 mg/kg) with low relative standard deviation values (0.63%–8.68%) were validated. The limits of detection and quantification were within 0.2–0.8 and 20 μg/kg, respectively. This study could provide guidance for the reasonable use of this fungicide and for the establishment of maximum residue level.
研究领域:
食品科学
·
分析化学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）