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
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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
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
TALANTA
·
2023
·
IF 6.1
Simin Chen,Yiqi Qie,Zhendong Hua,Haoyue Zhang,Youmei Wang,Bin Di,Mengxiang Su
Phytocannabinoids and their synthetic analogs (natural and synthetic cannabinoids) are illicit drugs that are widely abused worldwide. Wastewater-based epidemiology (WBE) is an objective approach for the estimation of population-level exposure to a wide range of substances, especially drugs of abuse. However, the concentrations of cannabinoids in wastewater are extremely low (frequently at the levels of nanograms per liter), and the existing pretreatment procedures for wastewater have the disadvantages of time-consumption or low extraction recoveries. This study aimed to propose a novel poly (methacrylic acid- co -ethylene glycol dimethacrylate)-functionalized polydopamine-coated Fe 3 O 4 nanoparticle (Fe 3 O 4 @ [email protected] (MAA- co -EGDMA)) as an adsorbent, and provide a highly sensitive quantitative analytical technique for the detection of five synthetic cannabinoids (SCs: 5 F-EDMB-PINACA, FUB-APINACA, MDMB-4en-PINACA, MDMB-FUBINACA, and PB-22) and one cannabis-related human metabolite (THC-COOH) in wastewater. The magnetic adsorbents were fully characterized by transmission electron microscopy (TEM), infrared spectroscopy (IR), vibrating sample magnetometry (VSM) and X-ray photoelectron spectroscopy (XPS). Subsequently, an MSPE-UHPLC-MS/MS method was developed and validated for the determination of six trace analytes in wastewater. The validation results showed that the method has limits of quantification as low as 0.1–1.0 ng/L. Additionally, the recoveries ranged from 62.81 to 124.02%, and the relative standard deviations (RSDs) of intraday and interday precision were less than 15%. This MSPE-UHPLC-MS/MS method was successfully applied to real wastewater samples, and the whole analytical process of one sample from pretreatment to the obtained quantitative results was completed in less than 30 min. Thus, the proposed method based on Fe 3 O 4 @ [email protected] (MAA- co -EGDMA) is a convenient, rapid, sensitive and reliable method for the determination of trace psychoactive drugs in wastewater.
研究领域:
分析化学
·
环境科学
·
纳米技术
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2020
·
IF 3.209
Zhipeng Wang,Hong Jiang,Xujiao Chen,Xinhua Song,Fengjing Xu,Fangchao Chen,Zhiguo Mao,Shouhong Gao,Wansheng Chen
A simple, rapid, reliable and sensitive ultra-high performance liquid chromatography tandem spectrometry (UHPLC-MS/MS) method was established for determination of eight serum protein-bound uremic toxins (hippuric acid, indoxyl sulfate, indole-3-acetic acid, kynurenic acid, L-kynurenine, melatonin, 3-carboxy-4-methyl-5-propyl-2-furanpropionic acid, 4-hydroxyhippuric acid) in serum from chronic kidney disease (CKD) dialysis patients. The chromatographic separation was achieved on an Atlantis T3 column (3 μm, 2.1 mm × 100 mm) using a gradient elution with acetonitrile (phase B) and 0.1% formic acid and 10 mmol/L ammonium acetate aqueous solution (phase A). The flow rate was 0.3 mL/min with analytical time of 5 min. The pretreatment procedure was developed with a simple protein precipitation and the hydrochlorothiazide was used as internal standard. The calibration ranges were set as 156.250-20000.000 ng/mL for indoxyl sulfate, hippuric acid, 3-carboxy-4-methyl-5-propyl-2-furanpropionic acid; 78.125-10000.000 ng/mL for L-kynurenine, indole-3-acetic acid and 4-hydroxyhippuricacid; 1.562-200.000 ng/mL for kynurenic acid; 0.078-10.000 ng/mL for melatonin. The UHPLC-MS/MS method for quantification of eight protein-bound uremic toxins was successfully developed and validated, and its clinical practicability was assessed on 81 serum samples from CKD patients.
研究领域:
分析化学
·
临床化学
·
肾病学
✓ 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
Shiqian Gao,Yiqiu Wu,Siyuan Xie,Zichun Shao,Xiumin Bao,Yumeng Yan,Youyi Wu,Junxia Wang,Zhanen Zhang
The ionic liquid (IL) was introduced to the synthesis system of magnetic zeolite imidazolate framework-8 (M/ZIF-8), which was benefit to the formation of binary imidazole and the co-modification of M/ZIF-8. The morphology and textural properties of ILM/ZIF-8 were characterized by SEM, TEM , BET and BJH. The crystal structural shape and size of MZIF-8 was unvaried with the interventional of IL. The ILM/ZIF-8 was applied to the concentration and determination of aflaoxins (AFB 1 , AFB 2 , AFG 1 and AFG 2 ) in milk samples based on magnetic solid phase extraction (MSPE) coupled with ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The experimental parameters of the MSPE, including amount of ILM/ZIF-8, pH, type and amount of desorption solvent, extraction time and sample volume were investigated by a univariate method and orthogonal screening. The four AFs were concentrated from the 20 mL milk when 90 mg ILM/ZIF-8 was used as magnetic adsorbent. The extraction efficiency of AFs was higher than 80.0% within 15 min. The limits of quantitative and detection were 7.5–26.7 and 2.3–8.1 ng/L, respectively. The proposed method was applied to the determination of milk samples containing trace amounts of AFs and the recoveries ranged from 79.0% to 102.5%, with RSD below 7.7%.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Arabian Journal of Chemistry
·
2022
·
IF 6.212
Jing An,Xin Wang,Haojing Song,Tangjuan Zhao,Hongyan Ren,Weijun Kang,Zhanjun Dong,Lingmei Niu,Hongmei Shi
A magnetic solid-phase extraction technique based on magnetic dendritic structured nanoparticles (Fe 3 O 4 @SiO 2 -NH 2 -G5) as adsorbent coupled with ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) has been developed to detect diazepam, midazolam, zolpidem, and zaleplon in human urine. With Fe 3 O 4 @SiO 2 -NH 2 as the central core, dendrimer (G5) grafted alternately with cyanuric chloride and imidazole were bonded to the surface of the core to synthesize Fe 3 O 4 @SiO 2 -NH 2 -G5. The morphology and structure of the magnetic materials were characterized by transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and dynamic light scattering (DLS). The key parameters affecting the extraction efficiency were optimized. A satisfactory performance was obtained under the optimum extraction conditions. The proposed method was validated, and the limits of detection of zaleplon, diazepam, zolpidem, and midazolam were 0.05, 0.05, 0.02, and 0.02 ng mL −1 , respectively. The linear correlation coefficients r of the four analytes were > 0.996, the intra-day precision was between 2.4 % and 9.4 % with the recoveries between 88.3 % and 104.8 %, and the inter-day precision ranged from 3.9 % to 15.2 % with the recovery in the range of 94.1 %−108.3 %. The magnetic dendritic structure nanomaterial Fe 3 O 4 @SiO 2 -NH 2 -G5 was successfully used to extract sedative-hypnotic drugs from human urine samples. The Fe 3 O 4 @SiO 2 -NH 2 -G5-based magnetic solid-phase extraction method eliminates centrifugation and filtration steps as in conventional extraction. Only one step of vortex dispersion extraction could achieve the separation and purification of the target compounds. The proposed method was simple, rapid, environment-friendly, and suitable for the analysis of sedative-hypnotic drugs in human urine.
研究领域:
分析化学
·
药物分析
·
纳米技术
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）