BIOMEDICAL CHROMATOGRAPHY
·
2024
·Vol. 39
·期 1
·e6055
·
IF 1.8
Jianhui Luo,Songshen Chen,WenYang Song,Yongtong Huang,Song Gao,Jiu Wang
Ethoxysanguinarine (ETSG), a benzophenanthridine alkaloid, exhibits diverse biological activities, including antibacterial, antifungal, anti-inflammatory, antioxidant, and anti-tumor effects. Despite these properties, limited research exists on ETSG in vivo pharmacokinetics due to its poor solubility and low bioavailability. In this study, we developed a rapid and specific UPLC-MS/MS method for ETSG bioanalysis. Sample preparation involved one-step protein precipitation using methanol and phellodendrine as an internal standard (IS). The Waters HSS T3 column (2.1 * 50 mm, 1.8 μM) employed a gradient elution with mobile phases A (2 mmol/L ammonium formate aqueous solution-formic acid [99.8:0.2, v/v]) and B (methanol-formic acid [99.8:0.2, v/v]). Mass analysis via Waters Q-mass spectrometer utilized positive scan mode and multiple reaction monitoring. ETSG and IS were detected at m/z 332.0 → 274.0 and 342.0 → 177.0, respectively, within 7.0 min. The method demonstrated excellent precision, accuracy, recovery, and stability, with a linear calibration curve (1.1–560 ng/mL) and strong correlation coefficient (0.9984). Successful pharmacokinetic evaluation in Sprague–Dawley rats included intravenous ETSG administration and intragastric ETSG nanoemulsion/suspension. This method enables steroidal saponin analysis from ETSG in biological samples.
研究领域:
药物分析
·
生物化学
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Food Chemistry-X
·
2024
·
IF 6.5
Yan Yang,Xin Li,Jian Lin,Rong Bao
Antibiotics and sedatives are used in freshwater fish culture and transportation, and residue in freshwater fish pose potential risks to human health. Therefore, a throughput method was developed to detect antibiotic and sedative residues in fish, simultaneously quantifying 68 antibiotics and 9 sedatives in freshwater fish using a modified QuEChERS extraction method and UPLC-MS/MS. Matrix-matched calibrations demonstrated good correlation coefficients (R 2 > 0.995), with a recovery range of 66.2–118.5%. The intra-day and inter-day relative standard deviation (RSD) were below 9.7% and 12.8%, respectively. The limits of detection (LOD) and quantification (LOQ) were 0.08–1.46 μg/kg and 0.25–4.86 μg/kg, respectively. 68.8% of analytes had weak matrix effects, and 13.0% had moderate matrix effects. In addition, diazepam and many types of antibiotics were detected in30 freshwater fish. The validation parameters were in agreement with the acceptable criteria of the Codex guidelines. The method was effective in analyzing antibiotic and sedative residues in freshwater fish.
研究领域:
食品安全
·
分析化学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2019
·Vol. 24
·期 17
·3117
·
IF 3.06
Mengqi Zhang,Xia Ren,Shijun Yue,Qing Zhao,Changlun Shao,Changyun Wang
Acanthus ilicifolius herb (AIH), the dry plant ofAcanthus ilicifoliusL., has long been used as a folk medicine for treating acute and chronic hepatitis. Phenylethanoid glycosides (PhGs) are one family of the main components in AIH with hepatoprotective, antioxidant, and anti-inflammatory activities. In this study, the pharmacokinetics of AIH was investigated preliminarily by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS). A simultaneously quantitative determination method for four PhGs (acteoside, isoacteoside, martynoside, and crenatoside) in rat plasma was first established by UPLC-MS/MS. These four PhGs were separated with an ACQUITY UPLC BEH C18column (2.1 × 50 mm, 1.7 μm) by gradient elution (mobile phase: MeCN and 0.1% formic acid in water, 0.4 mL/min). The mass spectrometry detection was performed using negative electrospray ionization (ESI−) in multiple reaction monitoring (MRM) mode. By the established method, the preliminary pharmacokinetics of AIH was elucidated using the kinetic parameters of the four PhGs in rat plasma after intragastric administration of AIH ethanol extract. All four PhGs showed double peaks on concentration-time curves, approximately at 0.5 h and 6 h, respectively. Their elimination half-lives (t1/2) were different, ranging from 3.42 h to 8.99 h, although they shared similar molecular structures. This work may provide a basis for the elucidation of the pharmacokinetic characteristics of bioactive components from AIH.
研究领域:
药理学
·
分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Saisai Ling,Ying Jin,Cuiyao He,Lisha Fu,Yuhua Deng,Xiaohui Qi,Zhenglei Wang,Yiying Wu
Tacrolimus is a potent macrolide immunosuppressant widely used in pediatric liver transplant patients. However, its narrow therapeutic window and significant inter-individual pharmacokinetic differences result in a poor correlation between blood concentrations and administered doses. To support its individualized dose, a sensitive, fast and robust ultra-high performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed to measure tacrolimus concentrations in whole blood of pediatric liver transplant patients. The method employed acetonitrile for protein precipitation, and sample separation was achieved using an Acquity UPLC CSH C 18 column (2.1 × 50 mm, 1.7 μm) with gradient elution. The mobile phase consisted of ammonium solution–water (0.5:1000, v /v) and methanol. The method demonstrated good linearity within a concentration range of 0.20–50.00 ng/mL. The intra- and inter-day precisions of tacrolimus in whole blood were less than 13.5 %, with the accuracy ranged from −7.2 % to 13.0 %. Selectivity, carryover, matrix effects, recovery, dilution reliability, and stability all met the standards set by relevant guidelines. The established UPLC–MS/MS method was successfully applied to measure the concentration of tacrolimus in the whole blood of pediatric liver transplant patients and support its individualized dose. Under the rapid UPLC–MS/MS method, 25 (65.8 %) patients required a dose increase, 3 (7.9 %) patients needed a dose reduction, and 10 (26.3 %) patients maintained their original dosage without adjustment.
研究领域:
药理学
·
临床医学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
Talanta Open
·
2025
·
IF 3.7
Xiao-Chen Huang,Shou-Lian Wei,Su Yao,Yu-Tong Lin,Jin-Kui Ma
This study developed a novel dummy molecularly imprinted polymer (DMIP) via emulsion polymerization for rapid, sensitive, and simultaneous detection of four fluoroquinolone (FQ) antibiotic residues in tilapia. The DMIP, coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), was thoroughly characterized for its structure and adsorption properties. Optimized parameters revealed a rough surface morphology with aggregated spherical structures (400-500 nm). Compared to a non-imprinted polymer (NIP), the DMIP exhibited faster adsorption kinetics and enhanced selectivity towards enrofloxacin and related FQ compounds. The DMIP-UPLC-MS/MS method achieved satisfactory recoveries (77-105%) for the four target FQs in tilapia, with intra-day and inter-day relative standard deviations of 3.6-9.2% and 4.0-11.7%, respectively. Method detection limits (LODs) ranged from 0.02-0.06 µg/kg, while quantification limits (LOQs) ranged from 0.06-0.2 µg/kg. This novel method demonstrates excellent potential for highly sensitive and selective monitoring of trace FQ residues in aquatic food products.
研究领域:
分析化学
·
食品安全
·
环境科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Yi Qin,Xiaojun Guan,Shichao Zhang,Zijie Zhang,Chenrong Huang,Liyan Miao
Almonertinib and anlotinib are tyrosine kinase inhibitors used to treat malignant tumors, with their combination currently applied to non-small cell lung cancer (NSCLC) patients. This study aimed to develop a simple and rapid UPLC–MS/MS method for simultaneously detecting almonertinib, its active metabolite HAS-719, and anlotinib in human plasma. The analytes were separated on a Waters HSST3-C18 column following protein precipitation with acetonitrile. Mass detection was performed on a Waters TQS triple quadrupole mass spectrometer under positive electrospray ionization mode. The MRM ions were m/z 526.5→71.96 for almonertinib, m/z 512.4 → 455.41 for HAS-719, m/z 408.16→ 339.03 for anlotinib and m/z 518.5→372.26 for d6-HAS-000719 (internal standard). Method validation followed FDA guidelines and Chinese Pharmacopoeia regulations, demonstrating acceptable accuracy, precision, matrix effects, recovery, and stability. The method showed excellent linearity over 0.5–500 ng/mL for all three analytes, with correlation coefficients (r²)≥ 0.99. The validated UPLC-MS/MS method successfully monitored almonertinib and anlotinib concentrations in clinical, particularly for NSCLC patients.
研究领域:
药理学
·
临床医学
·
肿瘤学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Ting Tai,Huan Zhou,Ting Zhu,Yu-Meng Jia,Jin-Zi Ji,Yi-Fei Li,Qiong-Yu Mi,Hong-Guang Xie
Vicagrel is a promising novel antiplatelet drug. However, the quantification of vicagrel in plasma is currently unavailable since it is liable to be hydrolyzed in plasma by esterases. In this study, an optimized strategy was developed and validated to stabilize vicagrel, 2-oxo-clopidogrel (thiolactone metabolite), and H4 (active thiol metabolite) before quantification of the analytes, such as addition of citric acid (for plasma acidification) and NaF (a non-specific esterase inhibitor) to inhibit esterase activity, immediate addition of a thiol-alkylating reagent MPB into blood samples to derivatize H4 for the formation of stable H4 derivative (i.e., MP-H4), use of the anticoagulant K 2 EDTA to minimize the conversion of 2-oxo-clopidogrel to H-endo, and keeping the analytes at 4 °C or on wet ice to minimize degradation of the analytes when processed and analyzed. The stability was measured as percent of each analyte remained in plasma samples after their storage for 4 h at 4 °C or in blood samples after 1 h at 4 °C. The results indicated that stability of vicagrel was increased significantly in stabilized plasma or blood samples compared with non-stabilized controls for rats and humans, respectively, and that the stability of 2-oxo-clopidogrel was increased to a certain extent. In contrast, MP-H4 formed was stable in plasma immediately after thorough mixture of MPB with blood. We conclude that the above strategy is useful for improving the stability of vicagrel, 2-oxo-clopidogrel, and H4 in rat or human plasma, and that vicagrel and its two major metabolites can be quantified accurately and simultaneously.
研究领域:
药理学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Frontiers in Chemistry
·
2022
·
IF 5.545
Shen Qing,Wang Haixing,Quan Bin,Sun Xiuhua,Wu Guohua,Huang Darong,Wang Qingcheng,Luo Pei
Salvia miltiorrhiza Bunge (SMB) has unambiguous biological functions in cardiovascular diseases, thus has been processed into different medicine forms. However, universal analytical method for fast quantification of bioactive compounds in SMB and SMB derived products is still missing. In this study, a polarity switching strategy was developed and optimized, which enabled the detection of the target compound in both positive and negative ion modes in a single run. The MS2 features of each compound were characterized to select the most prominent transitions for quantitative and qualitative analysis. Afterwards, the performance of this method was validated in terms of linearity (≥0.9916), limit of detection (LOD, 0.003–0.135 ngml−1), limit of quantification (LOQ, 0.010–0.450 ngml−1), precision (48.23 ± 2.58 ngml−1 to 53.72 ± 3.11 ngml−1), recovery (RSD 2.04%–5.79%), and stability (RSD ≤7.52%). Finally, the bioactive compounds in SMB and SMB derived products were determined, among which salvianate A, salvianolic acid A, and rosmarinic acid were the main components in all samples. In conclusion, the polarity switching UPLC-MS/MS method is efficient in accurate determining the bioactive compounds, which greatly shorten the time for analysis when compared with conventional methods. It has great potential quality control of SMB and SMB derived products.
研究领域:
药学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
American Journal of Translational Research
·
2021
·
IF 4.06
Shaochang Wu,Guidong Zhu,Dajin Zhou,Hongtao Xu,Longyou Zhao
Objective: This study was designed to demonstrate the accuracy of ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) in detecting serum concentration of anti-schizophrenic drugs in patients with mental illness. Methods: The study participants were 186 schizophrenia patients treated in our hospital. Serum concentrations of anti-schizophrenic drugs in Chinese patients with mental illness were evaluated according to the reference intervals of drug therapy recommended in the guidelines. Results: Five drugs, namely Aripiprazole (ARI), Amisulpride (AMI), Olanzapine (OLA), Paliperidone (PAL) and Ziprasidone (ZIP) all showed good linearity within the linear range. The within-day precision of the above five drugs was all between 1.3%-8.9% and the inter-day precision was between 1.8%-7.6%, with within-day and inter-day relative standard deviations (RSDs) less than 15.00% and accuracy ranging from 87.00% to 106.73%. However, AMI had a mean blood concentration of 436.31±241.05 ng/mL (median concentration: 379.34 ng/mL), which was significantly higher than the reference range (100-320 ng/mL) recommended in the guidelines. Good recovery rates (86.21%-99.77%) were obtained after the samples were stored at room temperature for 24 h, at 4°C for 48h and at -20°C for half a year. Conclusions: Given that UPLC-MS/MS renders more accurate results in detecting the concentration of psychotropic drugs, it can be applied clinically to detect the concentration of therapeutic drugs in patients with mental illness.
研究领域:
临床医学
·
药理学
✓ 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
Yingyue Yi,Guanghui Ren,Ming Zheng,Di Zhao,Ning Li,Xijng Chen,Yang Lu
JJH201501, a deuterated modification for multi-target antidepressant vortioxetine, is currently in phase I clinical trial. This study aimed to establish a sensitive and rapid UPLC-MS/MS method that was capable of simultaneously detecting JJH201501 and its major metabolite JJH201501-01 quantitatively in human plasma. The pretreatment was achieved by protein precipitation using 4-fold(v:v) acetonitrile with 5 ng/mL fluoxetine as internal standard precipitant. For method validation, the method was investigated in terms of the selectivity, inter- and intra-run precision and accuracy, carryover, matrix effect, extraction recovery and stability. The total running time was 3 min, and the retention time of JJH201501 and JJH201501-01 was 1.17 min and 1.05 min, respectively. The linear concentration range for JJH201501 and JJH201501-01 was 0.2 to 50 ng/mL and 0.4 to 100 ng/mL, respectively. The results showed that this method was in line with the guidelines for bioanalytical method proposed by FDA. In addition, the method was successfully applied to a plasma pharmacokinetic study of JJH201501 tablets in healthy volunteers which was part of the phase I trial.
研究领域:
药物分析
·
临床药理学
·
分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2018
·
IF 2.441
Yao Li,Sheng Guo,Tingting Hua,Yanyan Wang,Dandan Wei,Ming Zhao,Shulan Su,Jin-ao Duan
The fruit of Ziziphus jujuba ( Jujubae Fructus ) has been used as food and crude drug for thousands of years. Although several chemical and biological studies have revealed triterpenic acid as the main bioactive constituent of Jujubae Fructus responsible for immune-regulatory activity, only few pharmacokinetic studies have been conducted. To comprehend the kinetics of triterpenic acids and promote their curative application, a sensitive and efficient ultra-performance liquid chromatography coupled with mass spectrometry method (UPLC-MS/MS) was established. UPLC-MS/MS was applied for the simultaneous determination of ceanothic acid, epiceanothic acid, pomonic acid, alphitolic acid, maslinic acid , betulinic acid , and betulonic acid in normal and immunosuppressed rat plasma samples. After sample preparation, chromatographic separation was performed on an Acquity UPLC BEH C 18 column (2.1 × 100 mm, 1.7 μm) with acetonitrile : methanol (1:1, v/v) and 0.5% ammonium acetate in water as mobile phase . The established method was validated and found to be specific, accurate, and precise for the seven triterpenic acids, and was successfully applied for the pharmacokinetic study of rat plasma samples. The results showed that the pharmacokinetic parameters (C max , T max , AUC 0–t , AUC 0–∞, and CLz/F) in the plasma samples of immunosuppressed rats were significantly different from those in normal rats, and might provide an insight for the clinical usage of triterpenic acids from Jujubae Fructus .
研究领域:
药理学
·
分析化学
·
中药学
✓ 已验证
DOI
PubMed
高影响因子
Drug Testing and Analysis
·
2014
·Vol. 7
·期 2
·150-157
·
IF 2.84
Xin Yao,Guisheng Zhou,Yuping Tang,Sheng Guo,Dawei Qian,Jin-ao Duan
Ginkgo biloba leaf extract has been widely used in dietary supplements and more recently in some foods and beverages. In addition to the well-known flavonol glycosides and terpene lactones, G. biloba leaves are also rich in nucleobases and nucleosides. To determine the content of nucleobases and nucleosides in G. biloba leaves at trace levels, a reliable method has been established by using hydrophilic interaction ultra performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (HILIC-UPLC-TQ-MS/MS) working in multiple reaction monitoring mode. Eleven nucleobases and nucleosides were simultaneously determined in seven min. The proposed method was fully validated in terms of linearity, sensitivity, and repeatability, as well as recovery. Furthermore, hierarchical clustering analysis (HCA) was performed to evaluate and classify the samples according to the contents of the eleven chemical constituents. The established approach could be helpful for evaluation of the potential values as dietary supplements and the quality control of G. biloba leaves, which might also be utilized for the investigation of other medicinal herbs containing nucleobases and nucleosides. Copyright © 2014 John Wiley & Sons, Ltd.
研究领域:
植物化学
·
分析化学
·
药学
✓ 已验证
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）