JOURNAL OF HAZARDOUS MATERIALS
·
2021
·
IF 10.588
Shuang Li,Jiping Ma,Gege Wu,Jinhua Li,Xiaoyan Wang,Lingxin Chen
A simple method based on magnetic solid-phase extraction (MSPE) was developed for the simultaneous extraction of eleven emerging aromatic disinfection byproducts (DBPs) in water samples coupled with ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) determination. A magnetic covalent-organic framework (COF) material, namely, Fe 3 O 4 @TpBD, was facilely synthesized and fully characterized, followed by an MSPE process. Several important MSPE parameters, such as the magnetic ratio, Fe 3 O 4 @TpBD amount and sample pH, were systematically investigated. Under optimal conditions, the limits of detection and quantification of this COF-MSPE-UHPLC–MS/MS method were as low as 0.07–1.81 ng/L and 0.24–5.99 ng/L, respectively. Good precision was obtained with relative standard deviations (RSDs) of 1.3–10.9% (intraday) and 4.3–15.9% (interday). Furthermore, the validated method was proven applicable to real water samples; for example, the recoveries were 86.8–115.1% for the secondary effluent, and several DBPs in swimming pool water were detected. Notably, the MSPE process required only 7 min, ensuring that the DBPs were relatively stable during the whole analysis process and that Fe 3 O 4 @TpBD demonstrated excellent reusability. The COF-based MSPE method with simplicity, rapidity and efficiency provided an ideal sample pretreatment alternative to determine trace DBPs in complex matrices.
研究领域:
环境科学
·
分析化学
✓ 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
·
2021
·
IF 3.205
Yue Zhang,Xiang-xiang Huo,Li-yuan Cheng,Meng-ying Chen,Lei Song,Ying-li Yu,Kun Zhou
β-Elemonic acid is one of the main active ingredients isolated from Boswellia carterii Birdw . which has been reported to exhibit potential anti-inflammatory and anti-cancer activities. There is few information about pharmacokinetics and tissue distribution of β-elemonic acid by now. In this study, an ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-MS/MS) method has been developed and validated to determine β-elemonic acid in rat plasma and various tissues after intragastric administration. Oleanolic acid was chosen as an internal standard (IS) and the plasma/tissue samples were pretreated with one-step liquid–liquid extraction. Chromatographic separation was accomplished on Eclipse Plus C18 analytical column (2.1 × 50 mm, 1.8 μm) utilizing a gradient mobile phase system consisting of water (with 0.1% ammonia-solution) and acetonitrile. β-Elemonic acid and IS were detected and quantified using negative electrospray ionization in multiple reaction monitoring (MRM) mode with transitions of m / z 453.3 → 423.5 for β-elemonic acid and m / z 455.3 → 407.6 for IS. β-Elemonic acid showed good linearity over the investigated concentration range (r > 0.9934) in rat plasma and tissue sample. The method was successfully applied for determination of β-elemonic acid in bio-samples. A bimodal phenomenon appeared in the plasma concentration–time curve of the β-elemonic acid. The highest tissue concentrations were found in the intestine including jejunum, ileum and colon.
研究领域:
药物分析
·
药理学
·
生物化学
✓ 已验证
DOI
PubMed
高影响因子
CURRENT PHARMACEUTICAL DESIGN
·
2024
·Vol. 30
·期 32
·2574-2585
·
IF 2.6
Yuanjian Wang,Ruixun Wang,Huijia Wang,Ran Liu,Kaishun Bi,Qing Li
BackgroundEssential hypertension is a common clinical disease and a risk factor for cardiovascular and cerebrovascular diseases. Olmesartan medoxomil, amlodipine, and hydrochlorothiazide are commonly used antihypertensive drugs. The aim of this study was to establish a robust UPLC-MS/MS method for the simultaneous determination of olmesartan medoxomil, amlodipine, and hydrochlorothiazide in dog plasma. At the same time, the in vivo and in vitro release studies were conducted, and a preliminary in vitro-in vivo correlation (IVIVC) evaluation was performed.MethodsThe bioequivalence experiment was conducted with a double-crossed design. Three major components were extracted and analyzed by UHPLC-MS/MS. With the MRM scan, olmesartan and amlodipine were quantified by fragment conversion (m/z 447.10→190.10) and (m/z 408.95→294.00) under positive ESI mode, while hydrochlorothiazide was quantified with fragment conversion (m/z 295.90→268.90) under negative ESI mode. The in vitro release studies were performed using a USP paddle, and the dissolution medium was chosen from pH 6.0 to pH 6.8 according to the BCS classification of compounds. The IVIVC was calculated using the Wagner-Nelson equation.ResultsThe linear ranges of olmesartan, amlodipine, and hydrochlorothiazide in the plasma were 5.0-2500, 0.1-50, and 3.0-1500 ng/mL, respectively. All accuracies were within 3.8% of the target values, and the findings revealed that intra-day and inter-day accuracies were less than 12.1%. Moreover, the recoveries exceeded 88.3%, the matrix effect tests were positive, and the stability tests were positive. With the establishment of correlation, the distinguishable dissolution condition (pH 6.8) was selected as the predictable condition.ConclusionThe established method was suitable for the preclinical pharmacokinetic study of tripartite drugs with strong specificity and high sensitivity. Through the evaluation of IVIVC, the connection between in vivo and in vitro drug testing was initially established.
研究领域:
药理学
·
分析化学
·
临床医学
✓ 已验证
DOI
PubMed
高影响因子
TALANTA
·
2016
·
IF 4.035
Na Wei,Xian-En Zhao,Shuyun Zhu,Yongrui He,Longfang Zheng,Guang Chen,Jinmao You,Shu Liu,Zhiqiang Liu
This paper, for the first time, reported a simple, rapid, sensitive and environmental friendly ultrasonic-assisted in situ derivatization-dispersive liquid–liquid microextraction ( in situ UAD-DLLME) method followed by ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for the simultaneous determination of dopamine (DA), serotonin (5-HT) and their biosynthesis precursors and metabolites in rat brain microdialysates. In this work, a commercial reagent, Lissamine rhodamine B sulfonylchloride (LRSC), was proposed as a derivatization reagent. The ionization efficiency of neurotransmitters was greatly enhanced through the introduction of a permanent charged moiety of LRSC into their derivatives during electrospray ionization MS (ESI–MS) analysis. Parameters of in situ UAD-DLLME and UHPLC-MS/MS conditions were all optimized in detail. The optimum conditions of in situ UAD-DLLME were found to be as follows: a mixture of 150 μL of acetonitrile (dispersant) containing LRSC (derivatization reagents) and 50 μL of low toxic bromobenzene (extractant) was rapidly injected into an aqueous sample containing 30 μL of microdialysate and 800 μL of NaHCO 3 -Na 2 CO 3 buffer solution (pH 10.5) at 37 °C. After ultrasonication for 3 min and centrifuging for 2 min, the sedimented phase was conveniently injected for UHPLC–MS/MS analysis. Under the optimized conditions, good linearity was observed with the limits of detection (LODs, S/N>3) and limits of quantification (LOQs, S/N>10) in the range of 0.002–0.008 and 0.015–0.040 nmol/L, respectively. Meanwhile, it also brought good results of precision (3.2–13.0%, peak area RSDs %), accuracy (86.4–112%), recovery (73.9–105%), matrix effect (86.2–105%), and stability (3.1–8.8%, peak area RSDs %). The developed method was successfully applied for the simultaneous determination of multiple neurotransmitters, their precursors and metabolites in brain microdialysates of normal and L -DOPA induced dyskinesias (LID) rats.
研究领域:
神经科学
·
分析化学
·
药理学
✓ 已验证
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2023
·Vol. 415
·期 27
·6771-6783
·
IF 4.3
Ma Wanwan,Chen Huan,Hou Hongwei,Hu Qingyuan,Bai Yu
Phosphatidylcholine (PC) and lysophosphatidylcholine (LPC), two types of phospholipids (PLs), have been reported to be closely correlated with head and neck cancers of laryngeal cancer (LC) and thyroid cancer (TC), which make their analysis crucial. TiO 2 @COF-based solid-phase microextraction (SPME) coupled to UHPLC-MS/MS was developed for the rapid and accurate detection of seven potential PL biomarkers from small amounts of serum in this work. The combination of TiO 2 and COF proves to be effective for the extraction of the target analytes. Under optimal conditions, the developed TiO 2 @COF-based SPME-UHPLC-MS/MS method revealed good linearity ( R 2 ≥ 0.997) with LODs ranging from 0.05 to 0.38 ng/mL for PLs, the extraction recoveries and matrix effects ranging from 83.09–112.03% and 85.38–113.67%, respectively. As a high-throughput pretreatment method, satisfactory probe-to-probe reproducibility rates of 2.7–10.1% were obtained. Finally, the TiO 2 @COF-based SPME-UHPLC-MS/MS method was applied to analyze LPC 14:0, LPC 16:0, LPC 18:0, LPC 18:1, LPC 19:0, PC 16:0/18:1, and PC 18:0 in serum samples from early LC patients ( n = 15), early TC patients ( n = 15), and healthy volunteers ( n = 15). The results indicated that cancer patients could be effectively differentiated from healthy controls using orthogonal partial least squares discriminant analysis (OPLS-DA). In conclusion, the established TiO 2 @COF-based SPME-UHPLC-MS/MS method is reliable for the rapid determination of the seven PLs in serum samples, which is promising for early diagnosis of head and neck cancers. Graphical abstract
研究领域:
分析化学
·
肿瘤学
·
医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Shuai Yuan,Yangjiayi Xiang,Lizhu Chen,Ping Xiang,Yan Li
The quantification of illicit drugs in wastewater has become a valuable tool for monitoring illicit drug abuse. The commonly utilized methods for detecting drugs in wastewater require a substantial sample volume, extended pretreatment durations, and intricate procedures. This study first employed polydopamine-coated magnetic nanocomposites as adsorbents for magnetic solid-phase extraction, combined with UPLC-MS/MS, to simultaneously determine the concentrations of eleven common illicit drugs in wastewater. The synthesis process for Fe 3 O 4 @PDA is straightforward and high-yield. Benefiting from the strong magnetic response, good dispersibility, and abundant binding sites of the prepared nanocomposites, the extraction of illicit drugs from wastewater could be achieved in just 15 min. The method exhibited satisfactory limits of quantitation (ranging from 5 to 10 ng/L), commendable accuracy (ranging from 90.59 % to 106.80 %), good precision (with RSDs below 10 %), and less sample consumption (only 1 mL). The efficacy of this method was successfully validated through its application to actual wastewater samples collected from ten wastewater treatment plants. The results indicated that morphine, codeine, methamphetamine, and ketamine were the predominant illicit drugs present in the samples. The method developed is able to meet the needs of common illicit drug monitoring and high-throughput analysis requirements.
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2018
·
IF 2.831
Zhe Wang,Wei Sun,Zheng-Feng Lin,Rui Sun,Cheng-Ke Huang,Wei-Jian Ye,Yao-Yao Dong,Xiao-Dan Zhang,Rui-Jie Chen
Drug-drug interactions (DDIs) are thought to be associated with the inhibition of cytochrome P450 activities. The cocktail method with analysis of the metabolism of two or more probe drugs is used to determine CYP450 activities. In this study, we established a UHPLC-MS/MS method for simultaneous quantitation of four CYP450 probe drugs (phenacetin, omeprazole, metoprolol and midazolam) and their metabolites (acetaminophen, 5′-hydroxy omeprazole, α-hydroxy metoprolol and 1′-hydroxy midazolam) in rat plasma. Sample preparation by plasma protein precipitation was combined with a liquid-liquid extraction method. The separation was carried out on a ZORBAX Eclipse Plus C18 Rapid Resolution High Definition column with a gradient elution, using water containing 0.1% formic acid (A) and acetonitrile (B) in a run time of only 3.0 min. Detection was conducted with a 6420 series triple-quadrupole tandem mass spectrometer, using ESI in positive ion mode with multiple reaction monitoring (MRM). The calibration curves were linear over the concentration range 10–5000 ng/mL for phenacetin, omeprazole, metoprolol and midazolam, and 1–500 ng/mL for their metabolites. Intra- and inter-day precisions were within 15%, and the accuracies were in the range of 87–112%. The method was successfully applied to the pharmacokinetic study of probe drugs/metabolites and DDIs with 3-n-butylphthalide (NBP) after administration of a single oral dose of phenacetin, omeprazole, metoprolol and midazolam in rats.
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
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Ling Xin,Mengxin Ren,Yanwei Lou,Huawen Yin,Feng Qin,Zhili Xiong
Gushudan (GSD) was a traditional Chinese prescription with the remarkable effect of kidney-tonifying and bone-strengthening. However, the potential prevention mechanisms of the GSD on kidney-yang-deficiency-syndrome (KYDS) and its regulation on gut microbe metabolism still need to be further systematically investigated. This study established untargeted urinary metabolomics based on RP/HILIC-UHPLC-Q-Orbitrap HRMS and combined with multivariate statistical analysis to discover differential metabolites and key metabolic pathways. And the gut microbe metabolism pathway-targeted metabolomic based on HILIC-UHPLC-MS/MS was developed and validated to simultaneously determine 15 gut microbe-mediated metabolites in urine samples from the control group (CON), KYDS model group (MOD), GSD-treatment group (GSD) and positive group (POS). The results showed that a total of 36 differential metabolites were discovered in untargeted metabolomics. These differential metabolites included proline, cytosine, butyric acid and nicotinic acid, which were primarily involved in the gut microbe metabolism, amino acid metabolism, energy metabolism and nucleotide metabolism. And GSD played a role in preventing KYDS by regulating these metabolic pathways. The targeted metabolomics found that the levels of 10 gut microbe-mediated metabolites had significant differences in different groups. Among them, compared with the CON group, the levels of lysine, tryptophan, phenylacetylglycine and hippuric acid were increased in the MOD group, while the levels of threonine, leucine, dimethylamine, trimethylamine, succinic acid and butyric acid were decreased, which verified the disorders of gut microbe metabolism in the KYDS rats and GSD had a significant regulatory effect on this disorder. As well as by comparing analysis, it was found that the experimental results were consistent with previous metabolomics and microbiomics of fecal samples. Therefore, this integrated strategy of untargeted and targeted metabolomics not only elucidated the potential prevention mechanism of GSD on KYDS, but also provided a scientific basis for GSD preventing KYDS via the “gut-kidney” axis.
研究领域:
药理学
·
代谢组学
·
中医药
·
系统生物学
·
肠道微生物学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2016
·
IF 4.035
Xiuna Jia,Pan Zhao,Xiu Ye,Lianjun Zhang,Ting Wang,Qinyu Chen,Xiaohong Hou
As a novel material, metal-organic framework/graphite oxide (MIL-101(Cr)@GO) has great potential for the pretreatment of trace analytes. In the present study, MIL-101(Cr)@GO was synthesized using a solvothermal synthesis method at the nanoscale and was applied as sorbent in the dispersive micro-solid phase extraction (DMSPE) for the enrichment of the trace sulfonamides (SAs) from milk samples for the first time. Several experimental parameters including kinds of sorbents, the effect of pH, the amount of MIL-101(Cr)@GO, ionic strength , adsorption time, desorption solvent and desorption time were investigated. Under the optimal conditions, the linear ranges were from 0.1 to 10 μg/L, 0.2–20 μg/L or 0.5–50 μg/L for the analytes with regression coefficients ( r ) from 0.9942 to 0.9999. The limits of detection were between 0.012 and 0.145 μg/L. The recoveries ranged from 79.83% to 103.8% with relative standard deviations (RSDs)<10% ( n =3). MIL-101(Cr)@GO exhibited remarkable advantages compared to MIL-101(Cr), MIL-100(Fe), activated carbon and other sorbent materials used in pretreatment methods. A simple, rapid, sensitive, inexpensive and less solvent consuming method of DMSPE-ultra-high performance liquid chromatography-tandem mass spectrometry (DMSPE-UHPLC-MS/MS) was successfully applied to the pre-concentration and determination of twelve SAs in milk samples.
研究领域:
分析化学
·
食品安全
·
药物检测
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2021
·Vol. 413
·期 15
·3975-3986
·
IF 4.157
Liu Danyang,Yang Jina,Jin Wenbin,Zhong Qisheng,Zhou Ting
Pseudotargeted analysis combines the advantages of untargeted and targeted lipidomics methods based on chromatography-mass spectrometry (MS). This study proposed a comprehensive pseudotargeted lipidomics method based on three-phase liquid extraction (3PLE) and segment data-dependent acquisition (SDDA). We used a 3PLE method to extract the lipids with extensive coverage from biological matrixes. 3PLE was composed of one aqueous and two organic phases. The upper and middle organic phases enriched neutral lipids and glycerophospholipids, respectively, combined and detected together. Besides, the SDDA strategy improved the detection of co-elution ions in the lipidomics analysis. A total of 554 potential lipids were detected by the developed approach in both positive and negative modes using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Compared with the conventional liquid-liquid extraction (LLE) approaches, including methyl tert-butyl ether (MTBE) and Bligh-Dyer (BD) methods, 3PLE combined with SDDA significantly increased the lipid coverage 87.2% and 89.7%, respectively. Also, the proposed pseudotargeted lipidomics approach exhibited higher sensitivity and better repeatability than the untargeted approach. Finally, we applied the established pseudotargeted method to the plasma lipid profiling from the depressed rats and screened 61 differential variables. The results demonstrated that the pseudotargeted method based on 3PLE and SDDA broadened lipid coverage and improved the detection of co-elution ions with excellent sensitivity and precision, indicating significant potential for the lipidomics analysis. Graphical abstract
研究领域:
分析化学
·
药理学
·
神经科学
·
生物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Zhiquan Wang,Zhe Wang,Miao Lin,Bowen Zheng,Jinlan Zhang
Hyperlipidemia is a global metabolic disorder characterized by dysregulation of lipid metabolism. This dysregulation is closely associated with the altered homeostasis of cholesterol-cholesteryl ester (CE) metabolism in systemic circulation , and some organs. Additionally, the relationship between oxidized cholesteryl ester (oxCE) and the disease has also gained attention. Currently, there is a lack of comprehensive research on the alterations in cholesterol-CE metabolism in the context of hyperlipidemia, as well as the characteristics of lipid-lowering agents in regulating this metabolic state. Therefore, 40 oxCEs were identified in the hamster liver sample, and novel ultrahigh performance liquid chromatography−tandem mass spectrometry (UHPLC-MS/MS) methods were established for simultaneous analysis of cholesterol, 57 CEs, and 40 oxCEs in the serum, liver, adipose tissue, and intestine of hyperlipidemic hamsters. This study investigated the metabolic alterations between cholesterol-CE/oxCE in hyperlipidemic hamsters and those treated with lipid-lowering agents, including the Niemann-Pick-C1 like-1 protein (NPC1L1) inhibitor ezetimibe and the acyl coenzyme A : cholesterol acyltransferase (ACAT) inhibitor avasimibe . The study findings demonstrate metabolic disorders in cholesterol-CE/oxCE homeostasis in hyperlipidemic hamsters. Lipid-lowering agent therapy can improve the metabolic dysregulation caused by hyperlipidemia, with distinct characteristics: ezetimibe is more effective in reducing cholesterol, while avasimibe is more effective in reducing CEs/oxCEs. Eight potential biomarkers indicating the dysregulation of cholesterol-CE metabolism caused by hyperlipidemia and its improvement by lipid-lowering agents have been identified in the serum. This study offers new insights into the hyperlipidemia pathophysiology and the mechanisms of lipid-lowering agents from a novel perspective on cholesterol-CE/oxCE metabolic homeostasis.
研究领域:
代谢学
·
药理学
·
脂质组学
·
生物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
·
2023
·
IF 2.9
Zafar Iqbal Tanveer,Khurshid Ahmad,Ziliang Dong,Yong Chen,Xuesong Liu,Yongjiang Wu,Tenfei Xu
Poultry feed comprises cereals and their by-products and is vulnerable to aflatoxins contamination. This study utilised reduced graphene oxide–titanium dioxide (rGO–TiO2) nanomaterial as a dispersive solid phase extraction (d-SPE) adsorbent to extract, enrich and purify aflatoxins (aflatoxin B1, aflatoxin B2, aflatoxin G1 and aflatoxin G2). The synthesis of rGO–TiO2 nanomaterials through hydrothermal process and characterisation by transmission electron microscopy, scanning electron microscopy, Brunauer–Emmett–Teller (BET) and X-ray diffraction reveals that the nanomaterials have a single-layer structure embedded with TiO2 nanoparticles. The matrix-spiked technique was employed for the extraction process, optimisation of d-SPE, and analytical method validation. The most appropriate extraction solvent was acetonitrile/water/formic acid (79/20/1, v/v/v), with 30 min of extraction time assisted by ultra-sonication. The optimised d-SPE parameters were: 50 mg of rGO–TiO2 as sorbent amount, 2% methanol as the sample loading solvent, 30 min as adsorption time, and absolute ethanol as the washing reagent. The d-SPE method exhibited good desorption efficiency with 3 mL of acetonitrile/formic acid (99/1, v/v) and 20 min desorption time. After validation, the UHPLC–MS/MS analytical method has an acceptable range of specificity, linearity (R2 ≥ 0.999), sensitivity (LOQ 0.04–0.1 µg kg−1), recoveries (74–105% at three matrix-spiked levels) and precision (RSD 1.5–9.6%). Poultry feed samples (n = 12) were pretreated by this method to extract, enrich and analyse aflatoxins, which were detected in all poultry feed samples. The contamination levels were within the permissible limits.
研究领域:
分析化学
·
纳米技术
·
食品安全
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）