TALANTA
·
2019
·
IF 4.916
Qijun Wu,Jiaqi He,Hu Meng,Yu Wang,Yu Zhang,Hui Li,Liang Feng
Monitoring of copper(II) ion is critical for water safety. Herein, a solid phase extraction (SPE) column filled with home-made sulfonated PS-DVB microspheres was adopted to eliminate interference from other co-existing ions. Meanwhile, 1-(2-pyridylazo)-2-naphthol (PAN) as colorimetric reactant was dispersed in polyvinyl butyral (PVB) and immobilized on the filter paper. The as-fabricated paper-based microfluidic analytical device (μPAD) combined with home-made SPE column was utilized for the selective and quantitative determination of copper(II) ion. The selectivity and sensitivity for copper(II) ion were significantly enhanced by SPE-combined μPAD. The sensor has a noticeable color change in the presence of copper(II) ion. The limit of detection was as low as 0.340 μM, which is much less than the drinking water guidelines in many countries and organizations. This technology is convenient and does not need any expensive instrumentation and professional skills. It is easily used to achieve rapid and on-site assessment of copper(II) ion in real-world situations.
研究领域:
分析化学
·
环境科学
✓ 已验证
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Xinyuan Pei,Nan Zhang,Yuting Chen,Shiyu Miao,Huiyang Fu,Qingqing Zhu,Zhengbo Dai,Yi Chi,Ligang Hu,Rong Jin,Chunyang Liao
Antibiotics, as a typical class of emerging contaminants in the environment, are frequently detected at trace concentrations in various water samples. The chemical properties of antibiotics exhibit significant diversity, encompassing variations in molecular structure, amphoteric behaviour, and polarity. These differences present substantial challenges in developing universal detection methods for comprehensive monitoring of antibiotic contaminants. Therefore, it is imperative to develop more targeted, efficient, and sensitive analytical techniques. In this study, we develop a solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry (SPE-UHPLC-MS/MS) method. This method enables the simultaneous determination of 69 antibiotics divided into seven categories (tetracyclines, quinolones, sulfonamides, β-lactams, macrolides, lincosamides, and chloramphenicols) in surface water. The method achieved limits of detection (LOQs) ranging from 0.002 to 1.71 ng/L. The standard curves of the target compounds exhibited excellent linearity, with correlation coefficients (r 2 ) > 0.995, and most spiked recoveries fell within the range of 40.4–149 %, with relative standard deviations (RSDs) below 15 %. Using this method, 19 surface water samples from Qiantang River Basin, Zhejiang Province, China were analyzed, with 29 out of 69 analytes being detected (the total concentrations ranging from 5.69 to 131 ng/L). This method provides a reliable and robust analytical approach for the comprehensive monitoring of antibiotic contaminants in environmental water, offering critical insights for pollution control and water quality management efforts.
研究领域:
环境科学
·
分析化学
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产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2026
·
IF 4
Na Li,Ying-Jie Hao,Wanlu Mu,Jialin Duan,Xiaoli Wang,Ling-Xi Zhao,Hai-Long Jiang,Xiangfeng Chen,Yaqi Cai,Ru-Song Zhao,Xia Wang
Efficient monitoring of triazine herbicide residues is essential for safeguarding environmental and food safety. In this work, an innovative imidazolium-functionalized ionic conjugated microporous polymer (Im-CMP) was developed through Sonogashira–Hagihara coupling polymerization, and for the first time utilized as an adsorbent for solid-phase extraction (SPE) to enrich seven triazine herbicides from environmental water and fruit juice samples. Comprehensive characterizations confirmed that Im-CMP possessed a stable porous structure, high thermal stability, abundant π-π conjugated framework, and excellent hydrophilicity (water contact angle: 25.1°) derived from imidazolium ionic moieties, which solved the defect of poor aqueous dispersibility of traditional neutral CMPs. Density functional theory calculations and independent gradient model analysis revealed that the high extraction capacity of Im-CMP for triazine herbicides was dominated by efficient π–π stacking interactions, with synergistic contributions from directional weak interactions including C–H···π and N–H···π. Under optimized conditions, the established Im-CMP-SPE-HPLC-MS/MS method exhibited a wide linear range (0.25–250 ng·L⁻¹), low detection limits (0.03–0.11 ng·L⁻¹), high enrichment factors (387–554), and satisfactory recoveries (77.4–110.7%) with good precision. Additionally, the Im-CMP adsorbent demonstrated excellent reusability for nine cycles and consistent batch-to-batch reproducibility. This work not only provides a rational design strategy for ionic-functionalized porous adsorbents for sample pretreatment, but also establishes a sensitive, reliable and practical analytical method for the trace monitoring of triazine herbicides in complex environmental and food matrices, and further expands the application of ionic conjugated microporous polymers in the field of pesticide residue analysis.
✓ 已验证
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2026
·
IF 4.1
Yang Shuang,Wan Wei,Qu Ziyu,Yi Keke,Zhang Di,Jiang You,Ye Zihong,Fang Xiang,Xie Jie,Dai Xinhua
Steroid hormones play crucial regulatory roles in human growth, development, reproduction, and the maintenance of internal environmental homeostasis. Because the concentrations of most hormones in the body are extremely low and their chemical properties vary widely, developing an accurate and sensitive quantitative method has become a primary objective in clinical diagnostics. In this study, an isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) method was developed and validated for the simultaneous quantification of 22 steroid hormones in human serum. To enhance extraction and purification efficiency, a protein precipitation–solid-phase extraction (PP-SPE) approach was employed, forming a “dual purification” strategy. The limits of quantification for progesterone, cortisol, dihydrotestosterone, and dehydroepiandrosterone sulfate were 0.05, 0.50, 0.05, and 1.00 ng/mL, respectively, representing an improvement over previously reported values obtained using similar sample pretreatment methods. Method validation results demonstrated strong linearity for all 22 steroid hormones ( R 2 > 0.98). Accuracy ranged from 86.9% to 119.5%, intra-day precision was below 9.7%, inter-day precision was below 12.0%, and the matrix effect was controlled within 80.3%–118.1%. These findings indicate that the method is accurate, reliable, and suitable for analyzing multiple components in complex serum matrices. Twenty real serum samples were analyzed to evaluate the clinical applicability of the method. The results demonstrated that this method can be used clinically to monitor steroid hormone levels, assist in diagnosing and treating endocrine disorders, and provide a diagnostic basis for adrenal diseases. It holds significant reference value for clinical laboratory testing. Graphical
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Yuejiao Yang,Xitian Peng,Guiyou Chen,Huaming Xiao,Qiongwei Yu
Perfluorinated compounds (PFCs) are persistent in urban water systems, threatening the safety of drinking water and aquatic food chains. In this study, fluorinated loofah sponge (FLS) was prepared for selective solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) determination of 16 PFCs in urban water. The limits of detection (LODs) and limits of quantification (LOQs) of the established method (FLS-based SPE-LC-MS/MS) were 0.006–5 ng/mL and 0.01–10 ng/mL, respectively. This method exhibited a desirable precision with relative standard deviations (RSDs) less than 8.83 % and recoveries in the range of 85.4 %–107.2 %. Finally, this method was successfully applied to investigate the distribution of 16 PFCs in real urban water samples (such as tap water, bottled water, and lake water) collected in Wuhan, China, which enables sensitive dynamic monitoring of PFC migration in urban water networks and identification of potential sources so as to safeguard drinking water quality against emerging PFC contamination.
研究领域:
环境分析化学
·
环境污染与控制
·
水质安全
·
分析化学
·
环境健康
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2020
·
IF 6.306
Long Li,Ying Zhu,Feiyu Zhang,Hui Li,Jibran Iqbal,Ting Wu,Yiping Du
In this work, in-syringe membrane solid-phase extraction (MSPE) device was fabricated for the on-site sampling of sulfamethoxazole (SMX) in food samples followed by solid-phase fluorescence spectra analysis. The samples and fluorescamine (FA) were added to a syringe for derivation. Then, the derivative of SMX was extracted by a membrane in the syringe SPE device. Subsequently, the derivative on the membrane was measured immediately without additional elution procedure. The method was successfully applied in plasma, milk, and egg samples for the trace SMX detection, with the recovery of 98%–102%, RSDs from 1% to 6%. Compared with liquid chromatography, direct detection of the concentrated analyte significantly improved the sensitivity. Moreover, fluorescamine made it unnecessary to separate SMX from the interference. Consequently, it was a time-saving, low-cost, and easy-operation method, which demonstrated the potential of in-syringe SPE as a promising candidate for on-site analysis.
研究领域:
分析化学
·
食品安全
·
药物分析
✓ 已验证
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2013
·Vol. 37
·期 3
·257-264
·
IF 2.591
Qian Zhang,Tao Liang,Lingqing Wang,Yaqi Cai,Chukwunonso Peter Okoli
SPE using a cross-linked starch-based polymer (CSMDI) as an adsorbent for the determination of four nitrophenols at trace levels from aqueous solution was investigated. The CSMDI was synthesized from native starch using 4,4′-methylenebisphenyldiisocyanate as a cross-linking agent in dry DMF. Parameters affecting the extraction efficiency including the pH of the water sample, type of eluent and its volume, flow rate, sample volume, and methanol content were investigated and optimized. The optimized results exhibited excellent linear relationships ( R 2 > 0.995) for all the nitrophenols over the range of 2.0–200 ng/mL, with the RSD values in the range of 2.9–5.7% ( n = 5). The LODs ranged from 0.08–0.34 ng/mL (S/N = 3) for the four nitrophenols tested under optimum conditions. The developed method has been successfully applied for the analysis of several real environmental water samples including tap, river, and reservoir water. These results indicated that the CSMDI had a tremendous potential for the enrichment and determination of nitrophenols at trace levels in environmental water samples.
研究领域:
环境化学
·
分析化学
·
高分子科学
·
水质监测
✓ 已验证
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2012
·Vol. 36
·期 4
·789-795
·
IF 2.733
Ke-Jing Huang,Jing Li,Yan-Ming Liu,Lan Wang
The graphene functionalized with (3-aminopropyl) triethoxysilane was synthesized by a simple hydrothermal reaction and applied as SPE sorbents to extract trace polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. These sorbents possess high adsorption capacity and extraction efficiency due to strong adsorption ability of carbon materials and large specific surface area of nanoparticles, and only 10 mg of sorbents are required to extract PAHs from 100 mL water samples. Several condition parameters, such as eluent and its volume, adsorbent amount, sample volume, sample pH, and sample flow rate, were optimized to achieve good sensitivity and precision. Under the optimized extraction conditions, the method showed good linearity in the range of 1–100 μg/L, repeatability of the extraction (the RSDs were between 1.8 and 2.9%, n = 6), and satisfactory detection limits of 0.029–0.1 μg/L. The recoveries of PAHs spiked in environmental water samples ranged from 84.6 to 109.5%. All these results demonstrated that this new SPE technique was a viable alternative to conventional enrichment techniques for the extraction and analysis of PAHs in complex samples.
研究领域:
分析化学
·
环境科学
✓ 已验证
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2013
·
IF 2.591
Jiangmei Li,Haiyun Zhai,Zuanguang Chen,Qing Zhou,Zhenping Liu,Zihao Su
A novel method combining molecular imprinting and SPE was developed in a capillary column for the determination of auramine O in shrimp. The capillary monolithic column was prepared by UV-initiated in situ polymerization, using auramine O as template and methacrylic acid and ethylene dimethacrylate as functional monomer and cross-linker, respectively. The properties of the prepared capillary monolithic column were investigated under the optimized conditions coupled with HPLC, and then the morphologies of the inner polymers were characterized by SEM. The calibration curve was expressed as A = 103 C + 19.8 ( r = 0.9992) with a linear range of 0.25–25.0 μg/mL, and the recoveries of auramine O at different concentrations in shrimp ranged from 90.5 to 92.4% with RSDs ranging from 2.1 to 4.4%. The capacities of the molecularly imprinted polymer and nonimprinted polymer columns were 0.722 and 0.147 μg/mg, respectively, and the LOD (S/N = 3) of auramine O in shrimp was 17.85 μg/kg. Under the selected conditions, the enrichment factors obtained were higher than 70-fold. The results indicate that the prepared molecularly imprinted capillary monolithic column was reliable and applicable to the analysis of auramine O in shrimp.
研究领域:
分析化学
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2016
·Vol. 408
·期 13
·3527-3536
·
IF 3.125
Sun Yanan,Lv Zhengxian,Sun Zhiwei,Wu Chuanxiang,Ji Zhongyin,You Jinmao
A simple, sensitive, and selective high-performance liquid chromatography (HPLC) method using 9-(2-iodoethyl)acridone (IEA) as a novel fluorescence derivatizing agent for the simultaneous determination of six thiophenols has been developed. An efficient Pb 2+ -modified OASIS-MCX cartridge was used and could get good recoveries. IEA was successfully used to label thiophenols with high sensitivity and excellent selectivity. The effects of different solvents, pH, and surfactants on fluorescence properties of derivatives were investigated. To obtain the best labeling efficiency, derivatizing parameters including pH value, temperature, and concentration of IEA, as well as types of catalysts were also evaluated in detail. Under the optimal conditions, the separation could be achieved within 12 min with limits of detection (LODs) in the range of 0.6–5.8 μg L −1 and relative standard deviations (RSDs) < 3.9 %. This is the first time that IEA was applied to the analysis of thiophenols, and the established method has been successfully applied to the trace level detection of thiophenols in industrial wastewater samples.
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
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2024
·
IF 4
Jingwen Hao,Xuanxuan Fan,Naidong Chen,Ying Wang,Jun Xiao,Manman Zhang
A novel analytical method based on ultra-performance liquid chromatography-diode array detector (UPLC-DAD), solid-phase extraction (SPE), and quantitative analysis of multiple components by single marker (QAMS) was developed for the first simultaneous determination of 8 flavonoids in Pteridium aquilinum . The combination of QAMS and SPE demonstrated the convenient and economic advantages of the QAMS method while also exhibiting straightforward and cost-efficient advantages in terms of both the time and solvent usage of the SPE. The contents of the 8 flavonoids in P. aquilinum ranged from 0.59 to 697.08 μg/g. There were no substantial differences in the quantification when comparing the QAMS method and the external standard method (ESM). The standard deviations (SDs, %) obtained by QAMS and ESM were all less than 5 %. SPE increased the concentration of flavonoids by 4.18–18.9 times. The limits of detection (LODs) and quantification (LOQs) were in the ranges of 0.01–0.15 and 0.06–0.33 ng/g, respectively. Method validation revealed the linearity of the calibration curves (R 2 ≥ 0.9989), with recoveries between 97.02 % and 105 %, and the relative standard deviations (RSD) were all lower than 5 %. In addition, rhoifolin (4), apigenin (6), and amentoflavone (8) were first reported in P. aquilinum . The results suggested that this method was simple, reliable, and feasible for determining the flavonoids in P. aquilinum samples and could be further applied to various foods and herbal medicine samples.
研究领域:
植物化学
·
分析化学
·
药学
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产品关联
DOI
高影响因子
MOLECULES
·
2024
·Vol. 29
·期 12
·2856
·
IF 4.2
Qin Huang,Hua Zhou,Xianglun Wu,Jiaqi Jiang,Bingdong Zhan,Pinggu Wu
A promising method was established for the determination of nine halobenzoquinones (HBQs) in potable water by membrane solid-phase extraction (MSPE) pretreatment and the liquid chromatography–mass spectrometry (LC-MS) method. A 500 mL water sample was taken for enrichment by the SDB-RPS membrane, which was previously activated by methanol and ultrapure water. The sample was eluted with methanol and re-dissolved with the initial mobile phase after nitrogen blowing. Then, it was detected in negative ion mode using the working curve, and HBQs were quantified by the external standard method. The linearity was satisfactory in the concentration range of 4-1000 ng/L, with correlation coefficients of 0.9963~0.9994. The recoveries were 73.5~126.6% at three spiked levels, with relative standard deviations (RSDs) of 6.8~15.5%. The limits of detection (LOD, S/N = 3) values were 0.1~0.7 ng/L. The results demonstrate that the MSPE-LC-MS method is reliable, rapid, and sensitive for the simultaneous analysis of nine HBPs in potable water.
研究领域:
分析化学
·
环境科学
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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）