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TALANTA · 2023 · IF 6.1

Preparation of poly(methacrylic acid-co-ethylene glycol dimethacrylate)-functionalized magnetic polydopamine nanoparticles for the extraction of six cannabinoids in wastewater followed by UHPLC-MS/MS

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.

CAS / MDL: 78-67-1 97-90-5 79-41-4
研究领域: 分析化学 · 环境科学 · 纳米技术 · 药理学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2020 · IF 3.209

A rapid and sensitive method for simultaneous determination of eight protein-bound uremic toxins in human serum by UHPLC-MS/MS: application in assessing peritoneal dialysis

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.

CAS / MDL: 64-18-6
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
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npj Climate and Atmospheric Science · 2024 ·Vol. 7 ·期 1 ·1-8 · IF 8.5

Position-specific isomers of monohydroxy fatty acids in the land-atmosphere interface: identification and quantification

Niu Mutong,An Na,Zhang Wenxin,Hu Wei,Fu Xiaoli,Kawamura Kimitaka,Feng Yuqi,Zhu Quanfei,Fu Pingqing

Due to a wide variety and similar physicochemical properties of monohydroxy saturated fatty acids (OH-FAs) isomers as biomarkers, previously reported OH-FAs in environmental samples were mainly restricted to the α-, β-, (ω-1)- and ω-OH-FA isomers. Here, N,N -dimethylethylenediamine (DMED) labeling coupled with ultra-high-performance liquid chromatography-mass spectrometry (UHPLC-MS) analysis with multiple reaction monitoring mode (MRM) was developed to screen, identify and quantify position-specific isomers of OH-FAs (C8-C18). An identification strategy of positional isomers of OH-FAs, including α - , β - , 4 to (ω-2)-, (ω-1)- and ω-OH-FAs, was established by integrating the characteristics of peak intensity ratios of product ions based on the library of OH-FAs. Meanwhile, d 4 -DMED-labeled OH-FA standards as internal standards were adopted for the relative quantification of positional isomers. The extraction processes were optimized for different interface-environmental samples. Our method offers a promising tool to investigate position-specific isomers of OH-FAs in the land-atmosphere interface.

研究领域: 环境科学 · 分析化学 · 生物化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2019 · IF 2.813

Determination of aflatoxins in milk sample with ionic liquid modified magnetic zeolitic imidazolate frameworks

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%.

CAS / MDL: 64-18-6 693-98-1
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
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Arabian Journal of Chemistry · 2022 · IF 6.212

Simultaneous determination of four sedative-hypnotics in human urine based on dendritic structured magnetic nanomaterials

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.

CAS / MDL: 288-32-4
研究领域: 分析化学 · 药物分析 · 纳米技术
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JOURNAL OF SEPARATION SCIENCE · 2025 ·Vol. 48 ·期 8 ·e70253 · IF 2.8

Quantification and Aerodynamic Particle Size Distribution of Revefenacin Aerosol With UHPLC-MS/MS

Difeng Zhu,Jing Dou,Li Ping,Yawen Hong,Chao Chen,Chenxing Yuan,Qixiu Li,Wenjie Luo,Xiaoqing Chi

Aerosol inhalation therapy offers significant benefits in treating chronic obstructive pulmonary disease, including rapid onset of action and reduced systemic side effects. Revefenacin, a long-acting bronchodilator, has demonstrated efficacy in improving lung function and alleviating chronic obstructive pulmonary disease symptoms through aerosol delivery. However, quantitative methods for determining the inhaled concentration of revefenacin aerosol remain limited. This study developed and validated a rapid, robust ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method to quantify revefenacin aerosol concentration. The method, with an analysis time of 2 min, exhibited excellent specificity, precision, and a lower limit of quantification of 2 ng/mL. The aerosol extraction recovery averaged 98.5%. The method was successfully applied to assess aerosol concentration and aerodynamic particle size distribution under different sampling conditions. Results showed that after 15 min of nebulization, the average aerosol concentrations collected using syringe aspiration and impactor sampling methods were 0.98 and 0.95 mg/m 3 , respectively, demonstrating consistency between the techniques. Aerodynamic particle size distribution analysis revealed stable particle size distribution with atomization times of 5 and 15 min, yielding mass median aerodynamic diameters of 2.31 and 2.35 µm, fine particle fractions of 76.5% and 76.7%, and geometric standard deviations of 2.44 and 2.41, respectively. These findings indicate that the aerodynamic properties of revefenacin aerosol remain stable over prolonged nebulization. This study establishes a reliable analytical method for revefenacin aerosol quantification and provides valuable insights into its aerodynamic characteristics, supporting its further application in chronic obstructive pulmonary disease treatment.

CAS / MDL: 64-18-6
研究领域: 药物分析 · 肺部给药 · 分析化学 · 呼吸系统疾病
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2021 · IF 4.952

Phenolics in Citrus aurantium fruit identified by UHPLC-MS/MS and their bioactivities

Lingrong Wen,Mingyang He,Chunxiao Yin,Yueming Jiang,Donghui Luo,Bao Yang

Sour orange ( Citrus aurantium ) is a popular fruit with health benefits. Phenolics are the dominant bioactive compounds in this fruit. However, the full phenolics composition remains unclear. In this work, UHPLC-MS/MS was used to qualify and quantify the phenolics in sour orange fruits of cv. Morocco (MSO) and United (USO). Fifty-eight phenolics, including 26 flavonoid glycosides , 22 polymethoxylated flavonoids, 8 coumarins and 2 phenolic acids , were identified. Four limonoids were characterized. Flavonoid glycosides were the leading phenolics in MSO, while polymethoxylated flavonoids (including nobiletin, tangeritin and sinensetin) were dominant in USO. The phenolic extracts showed good antioxidant activities . USO extract had a significantly ( p  < 0.05) stronger neuroprotective activity than MSO extract. Auraptene, nobiletin and tangeritin were highly responsible for the neuroprotective activity. The results were helpful for the development of functional foods with sour orange.

研究领域: 食品科学 · 药理学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY A · 2022 · IF 4.601

Preparation and application of polystyrene-divinylbenzene sorbent with weak cation-exchange character for the selective extraction of illicit drugs in environmental water

Hongyu Ning,Yilei Fan,Huijun Liu,Zhongping Huang,Xing Ke,Yu Xu,Yuanbin She

A novel mixed-mode weak cation-exchange sorbent (PS-DVB-WCX-II) was prepared by the modification of polystyrene-divinylbenzene with mercaptosuccinic acid for the selective extraction of illicit drugs in environmental water. The PS-DVB-WCX-II was synthesized through the Friedel-Crafts acylation reaction on the surface of polystyrene-divinylbenzene, followed by nucleophilic substitution reaction and thiol-ene click reaction. The sorbent can selectively absorb illicit drugs through the reverse-phase interactions provided by benzene ring on the polymer backbone and the ion-exchange interactions provided by functional group (-COOH). As compared with the extraction performance of three commercial SPE cartridges, it was found that the prepared sorbent had better adsorption performance with the recovery values between 84.1% and 106.0% for the selected 11 illicit drugs under the optimized SPE conditions. Illicit drugs in environmental water were extracted by the sorbent, prior to the detection of UHPLC-MS/MS. Two quantitative methods were established respectively for the detection of 11 illicit drugs in different matrices of river water and wastewater. Both methods had good determination coefficient (r 2 >0.992) in the range of 0.5–50 ng/L, 2.5–250 ng/L, 5–500 ng/L, and low limits of detection ( S / N  = 3) of 0.17–1.67 ng/L. In the real wastewater samples, the concentration of morphine was 18.3–126.3 ng/L, and the methamphetamine was 12.7–27.4 ng/L. Meanwhile, PS-DVB-WCX-II was compared with Oasis MCX and Oasis HLB in the detection of real wastewater samples. The results revealed that PS-DVB-WCX-II and Oasis MCX had better performance in absorbing methamphetamine than Oasis HLB, and PS-DVB-WCX-II had better ability to remove the matrix. The results suggested that the prepared weak cation-exchange sorbent had the potential in the application of illicit drug detection in environmental water.

研究领域: 分析化学 · 环境科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Foods · 2026 ·Vol. 15 ·期 16 ·2855 · IF 6

Metabolomics Analysis of Different Varieties of Pouteria caimito Fruit Based on UHPLC-MS/MS

Haijie Huang,Li Zhao,Zhikai Wang,Yang Qiao,Huidong Deng,Yingjun Ye,Kaili Ding,Xuejie Feng,Yijun Liu

To investigate the differences in pulp metabolites among four varieties of Pouteria caimito fruit (JZL1, JZL3, JZL5, and JZL6), ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was employed for the separation and identification of metabolites. A total of 1285 metabolites were identified, including 648 in positive ion mode and 637 in negative ion mode. At the class level, carboxylic acids and derivatives (14.32%) and organooxygen compounds (11.83%) accounted for the highest proportions; at the subclass level, amino acids, peptides, and analogues (12.53%) as well as carbohydrates and carbohydrate conjugates (9.49%) were the main categories. PLS-DA analysis revealed significant differences in metabolite profiles among the four varieties, with numerous up-regulated and down-regulated metabolites in each comparison group, and some metabolites showed fold changes > 10 or <0.1. KEGG pathway enrichment analysis further indicated that differential metabolites were primarily enriched in pathways such as ABC transporters, citrate cycle (TCA cycle), starch and sucrose metabolism, and linoleic acid metabolism. This study provides an important metabolomic basis for variety identification, nutritional quality evaluation, and functional component development of Pouteria caimito fruit.

CAS / MDL: 1336-21-6
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Separation Science Plus · 2025 ·Vol. 8 ·期 6 ·e70069 · IF 1.6

Quantitative Determination of Six Cardiovascular and Cerebrovascular Drugs in Human Plasma by UHPLC-MS/MS

Yilin Li,Li Song,Yan Liang,Hui Li

QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) is a pretreatment technique based on dispersive solid-phase extraction. This study employs QuEChERS technology in preprocessing plasma samples, combined with high-performance mass spectrometry, to quantify the concentrations of six drugs (used in the treatment of cardiovascular and cerebrovascular diseases: butylphthalide, clopidogrel, rosuvastatin, ramipril, atenolol, and simvastatin). This method utilizes 3 mL of acetonitrile as a precipitant, 500 mg of anhydrous magnesium sulfate as a salt precipitation agent, and 10 mg of C18 as an adsorbent for treating plasma samples. Chromatographic separation was carried out using a Shim-pack GIST C18 from Shimadzu (2.1 × 100 mm; 2 µm), with a mobile phase consisting of 0.1% methanol and 0.1% water, detected in ESI positive ion mode. N -butylphthalide, clopidogrel, and rosuvastatin demonstrated linear relationships within the range of 1–100 ng/mL, while ramipril and atenolol exhibited linear relationships within the range of 2–200 ng/mL. Simvastatin exhibited linear relationships in the range of 4–400 ng/mL. All linear equations exhibit R 2 values exceeding 0.990, and the methodological validation results meet the requirements. The method offers the advantages of rapidity, simplicity of operation, and high accuracy, making it suitable for drug detection in patients with hypertension, hyperlipidemia, or stroke.

CAS / MDL: 64-18-6
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2016 · IF 2.687

Simple and fast determination of perfluorinated compounds in Taihu Lake by SPE-UHPLC–MS/MS

Pengfei Zhu,Xia Ling,Wenwei Liu,Lingcan Kong,Yuyang Yao

A simple and fast analytical method for determination of eleven Polyfluorinated Compounds (PFCs) in source water was developed in the present work. The water sample was prepared without filtered through microfiltration membrane and 500   mL of source water was enriched by the solid phase extraction (SPE). The targent compounds were analyzed by ultra high performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS). The optimized analytical method was validated in terms of recovery, precision and method detection limits (MDLs). The recovery values after correction with the corresponding labeled standard were between 97.3 and 113.0% for samples spiked at 5   ng/L, 10   ng/L and 20   ng/L. All PFCs showed good linearity and the linear correlation coefficient was over 0.99. The precisions were 1.0–9.0% (n   =   6). As the result of the enrichment, the MDL values ranged from 0.03 to 1.9   ng/L and were enough for analysis of the trace levels of PFCs in the Taihu Lake. The method was further validated in determining the source water and the results showed that PFHxS, PFHxA, PFOA and PFOS were the primary PFCs in Taihu Lake which might be different from the other researches. The method can be used for determination of PFCs in water with a stable recovery, good reproducibility, low detection limit, less solvent consumption, time saving and labor saving. To our knowledge, this is the first method that describes the effect of the filter membrane on the determination of PFCs in water which might acquire more accurate concentration of PFCs in Taihu Lake.

CAS / MDL: 631-61-8
研究领域: 环境科学 · 分析化学
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CHEMICAL ENGINEERING JOURNAL · 2019 · IF 8.355

Teamed boronate affinity-functionalized branched polyethyleneimine-modified magnetic nanoparticles for the selective capture of ginsenosides from rat plasma

Ningning Zhao,Zhiqiang Liu,Junpeng Xing,Zhong Zheng,Fengrui Song,Shu Liu

Boronate-functionalized materials have been widely used for the selective separation and enrichment of glycoproteins and glycans. However, emerging boronic acid materials either use expensive boronic acid compounds containing electron-withdrawing groups combined with a graft structure or explore only simple methods for the synthesis of boronic acid structures with improved electron-withdrawing groups. In this study, polyethyleneimine (PEI)-assisted teamed boronate affinity (TBA)-functionalized magnetic nanoparticles (MNPs) (Fe 3 O 4 @PEI@TBA NPs) were designed to specifically capture trace ginsenosides from rat plasma under neutral conditions without requiring protein precipitation. The synergistic effect of the Fe 3 O 4 @PEI@TBA NPs exhibited higher affinity for ginsenosides (45.64 mg g −1 ) based on PEI dendrimer-assisted multivalent binding, the low p K a value of TBA and specific recognition sites. Additionally, the captured ginsenosides were quickly detected and characterized using ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-MS) and an enriched in-house library. Compared to the 37 compounds identified using the methanol method, 63 ginsenoside prototypes and metabolites were successfully detected and identified in rat plasma by applying this novel integrated strategy. The strategy exhibited selectivity and identified more types and quantities of ginsenosides. Our study provided in-depth insight into the synergistic development of specific functional materials in combination with advanced analytical platforms for the selective capture and characterization of trace glycoconjugate families in analytical, engineering and biomedical fields under neutral conditions.

研究领域: 分析化学 · 生物医学 · 材料科学
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