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JOURNAL OF SEPARATION SCIENCE · 2025 ·Vol. 48 ·期 5 ·e70141 · IF 2.8

Materials Institute Lavoisier-68(Al)-coated Frosted Glass Rods for Enhanced Detection of Tetracyclines in Food Samples by Suspended Bar Sorptive Extraction

Tao Bao,Jiao Long,Jina Wang,Meng Sun,Xinglong Zheng,Sicen Wang

Herein, we present a sensitive analytical method utilizing Materials Institute Lavoisier (MIL)-68(Al)-coated frosted glass rods (MIL-68(Al)@FGR) coupled with ultra-high-performance liquid chromatography for detecting trace tetracycline (TC) antibiotics in food matrices. The synthesized coating was thoroughly characterized through field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy analyses. Systematic optimization of critical parameters, including extraction time, sample pH, formic acid concentration, and desorption time achieved optimal extraction efficiency. The developed method exhibited a wide linear range (3–70 ng/mL) with low detection limits (0.1–0.3 ng/mL) for target analytes. Practical application to spiked food samples demonstrated satisfactory recoveries of 75.2%–115.1% across milk, chicken, and egg matrices, accompanied by precise relative standard deviations of ≤8.4%. The MIL-68(Al)@FGR-based approach shows exceptional resistance to matrix interference and detection sensitivity, establishing an effective strategy for monitoring TC residues in complex food samples.

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
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TALANTA · 2017 · IF 4.162

Simultaneous determination of acidic phytohormones in cucumbers and green bean sprouts by ion-pair stir bar sorptive extraction-high performance liquid chromatography

Wei Wang,Man He,Beibei Chen,Bin Hu

A simple, sensitive and inexpensive method of ion-pair stir bar sorptive extraction (IP-SBSE) combined with high performance liquid chromatography -ultraviolet (HPLC-UV) detection was developed for the simultaneous determination of three acidic phytohormones (salicylic acid (SA), indole-3-acetic acid (IAA), and abscisic acid (ABA)) in vegetables. With the addition of cationic surfactant-cetyltrimethylammonium bromide (CTAB) in sample solutions, ion pair between CTAB and target phytohormones were formed, leading to an improvement of the extraction efficiency for target phytohormones by C 18 silica coated SBSE. The factors affecting the extraction efficiency of three target phytohormones by IP-C 18 coated SBSE were optimized, and the optimal experimental conditions were established. Under the optimal conditions, the limits of detection for SA, IAA and ABA obtained by IP-C 18 -SBSE-HPLC-UV were 2.7, 2.1 and 0.3   μg   L −1 , with the relative standard deviations of 6.0%, 5.0% and 8.3%, respectively, and the enrichment factor was 32–49-fold. The developed method was applied to the determination of SA, IAA and ABA in cucumbers and green bean sprouts, and the recoveries of SA, IAA and ABA for the spiked samples were between 72.8% and 109.5%.

研究领域: 分析化学 · 植物学
✓ 已验证 DOI 高影响因子
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ELECTROPHORESIS · 2024 · IF 3

Suspended Stir Bar Sorptive Extraction Based on Zr-MOF-Modified Cotton Thread for Enrichment and Detection of Three Trace Quinolones in Fish Tissue

Jiao Long,Yan Gao,Kangjia Sheng,Tao Bao,Sicen Wang

In this study, an efficient and practical method was established to enrich and detect three trace quinolones in fish tissue. Low-cost and environment-friendly cotton threads were coated with PCN-224 using a simple one-pot hydrothermal method. The PCN-224-modified cotton threads (PCN-224@CTs) were characterized to ensure that the crystal was successfully fabricated on the surface of cotton threads. The prepared PCN-224@CTs were wrapped around steel needles to form suspended bars. Key factors of extraction and desorption were optimized, and analytical performance was tested. Suspended bar sorptive extraction coupled with ultra-performance liquid chromatography (UPLC) with a photodiode array detector was used to analyze the quinolones in fish tissue. The detection limits of quinolones were 0.26–1.15 ng/mL, and the recoveries were achieved in the range of 81.31%–115.81%, indicating a simple method with high sensitivity and satisfactory practicability of enriching, separating, and detecting trace quinolones was successfully established.

CAS / MDL: 13520-92-8
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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ANALYTICA CHIMICA ACTA · 2020 · IF 5.977

Surface area expansion by flower-like nanoscale layered double hydroxides for high efficient stir bar sorptive extraction

Wei Zhou,Xuemei Wang,Chenlu Wang,Wenqing Li,Zilin Chen

Enhancing the surface area of stationary phase is essential in chromatographic science. In this work, nanoscale NiAl-layered double hydroxides (NiAl-LDHs) with flower-like structure was used as a platform for supporting the stationary phase. Then strong hydrophobic p-naphtholbenzein molecule was immobilized onto the LDHs layer as sorbent for stir bar sorptive extraction (SBSE). The flower-like LDHs layer significantly increased the extraction efficiency through increasing the specific surface area and immobilized amounts of stationary phase. In addition, the LDHs can also provide anion exchange ability, which expanded the application of this stir bar for analysis of not only hydrophobic but also anionic analytes. For improving the workability, a poly(ether ether ketone) (PEEK) jacket stir bar with detachable dumbbell-shaped structure was employed. The PEEK jacket with high mechanical strength and dumbbell-shaped structure improved the durability of stir bar and the detectable design allowed elution to be realized with less solvent that enhanced the enrichment factor. The proposed stir bar showed good performance for the extraction of multiple analytes including flavonoids , non-steroid anti-inflammatory drugs and chlorophenoxy acids. By coupling with high performance liquid chromatography-ultraviolet detection (HPLC-UV), the SBSE-HPLC-UV method was applied for the extraction of three active components including bavachin, isobavachalcone and bavachinin in Psoralea corylifolia L. herb with low limit detection of 0.01–0.02 ng/mL.

研究领域: 分析化学 · 材料科学
✓ 已验证 DOI PubMed 高影响因子
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2016 ·Vol. 408 ·期 19 ·5329-5335 · IF 3.125

Barbell-shaped stir bar sorptive extraction using dummy template molecularly imprinted polymer coatings for analysis of bisphenol A in water

Liu Ruimei,Feng Feng,Chen Guolin,Liu Zhimin,Xu Zhigang

This study reports the development of a novel dummy template molecularly imprinted polymer (MIP)-coated barbell-shaped stir bar. The MIP stir bar coatings were prepared by using 2,2-bis(4-hydroxyphenyl)butane (BPB), 4,4'-dihydroxydiphenylmethane (BPF), 4- tert -butylphenol (PTBP), and tetrabromobisphenol A (TBBA) as dummy templates using a capillary in situ polymerization method. Uniform coatings can be prepared controllably. The method is simple, easy, and reproducible. The barbell-shaped stir bar was developed by using medical silicone tubes as wheels. The wheels could be removed and reinstalled when necessary; therefore, the barbell-shaped stir bar was easy to disassemble and reassemble. The novel MIP-coated stir bar showed good selectivity for the target analyte, bisphenol A (BPA). The established method is selective and sensitive with a lower detection limit for BPA of 0.003 μg/L. The dummy template MIP-coated stir bar is suitable for trace BPA analysis in real environmental water samples without template leakage. The novel stir bar can be used at least 100 times.

CAS / MDL: 98-54-4 140-66-9
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
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CHROMATOGRAPHIA · 2017 ·Vol. 80 ·期 3 ·473-482 · IF 1.402

Novel Stir Bar Array Sorptive Extraction Coupled With Gas Chromatography–Mass Spectrometry for Simultaneous Determination of Three β2-Agonist Residues in Pork

Liu Haibo,Ousmane Diebate,Gan Ning,Wu Dazhen,Li Tianhua

Abstract This study aimed to simultaneously determine three β2-agonists (clenbuterol, salbutamol, and ractopamine) in pork samples using novel stir bar array sorptive extraction coupled with gas chromatography–mass spectrometry. Pencil refill was employed as the substrate of stir, which was covered with carboxyl graphene sheets and polyluminol coating. The coating was simply prepared by electrochemical deposition of luminol at a voltage of 0–0.6 V. Then, an automatic device with the stir bar array for extraction was used. The conditions for the extraction were optimized. Under the optimum extraction conditions, with toluene as the extraction solvent, the extraction and desorption times were 20 min. A good linearity of three β2-agonists was obtained in the range of 0.5–100 ng g −1 by gas chromatography–mass spectrometry detection. The recovery of clenbuterol, salbutamol, and ractopamine in spiked pork samples ranged from 88.7 to 93.2%, 85.5–94.2%, and 85.7–93.9%, respectively, with the relative standard deviations less than 10%. The detection limits were in the range of 0.022–0.091 ng g −1 for pork samples. The extraction coating with high extraction capacity was simply fabricated by the electrochemical method, which could simplify the pretreatment procedures. Moreover, the array could extract several samples simultaneously and improve the pretreatment efficiency. Graphical Abstract

研究领域: 食品科学 · 分析化学
✓ 已验证 DOI 高影响因子
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JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY · 2016 ·Vol. 16 ·期 12 ·12374-12381 · IF 1.338

Fabrication of Novel Stir Bar Sorptive Extraction Coating Based on Magnetic Molecularly Imprinted Polymer Through Atom Transfer Radical Polymerization for Trace Analysis of Estrogens in Milk

Qiu Xiuzhen,Wu Yan,Chen Dazhi,Lai Liangyang,Liang Yong,Guo Huishi

In this paper, we reported an effective method for the preparation of molecularly imprinted polymers (MIPs) on silica gel with diethylstilbestrol (DES) as template molecule through surface-initiated atom transfer radical polymerization (ATRP). A novel stir bar sorptive extraction (SBSE) coating was prepared based on MIPs by glass filling with magnetic core as substrate through sol–gel. The structure and morphology of MIPs were characterized by infrared spectroscopy (IR) and scanning electron microscope (SEM). In order to evaluate the usability of the MIPs-coating, a methodology by combining MIPs-SBSE with high performance liquid chromatography (HPLC) detection for the determination of DES, dienestrol (DS), hexestrol (HS) and bisphenol (BPA) in complex samples was developed. Parameters that influenced the extraction efficiency such as extraction time, desorption solvent and desorption time were optimized. The results show that under the optimum extraction conditions, the MIPs-coated stir bar showed better extraction capacity and good selectivity than that of non-imprinted polymers (NIPs) coated stir bar to DES and its analogues. The MIPs-coated stir bars could be used at least 5 times without reduce of extraction ability. The linear ranges were 1.0˜1000 μg/L for DES and BPA, 1.0˜400 μg/Land 10.0˜400 μg/L for DS and HS, respectively. The detection limits were within the range of 0.107˜0.786 μg/L. The recoveries of the spiked milk samples were within the range of 73.60˜96.30%, the RSDs were within 3.77˜8.96%. The developed method is simple, selective, sensitive and applicable for the analysis of trace estrogen in complicated samples.

研究领域: 分析化学 · 环境科学
✓ 已验证 DOI 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2016 · IF 3.926

Water-compatible graphene oxide/molecularly imprinted polymer coated stir bar sorptive extraction of propranolol from urine samples followed by high performance liquid chromatography-ultraviolet detection

Wenying Fan,Man He,Linna You,Xuewei Zhu,Beibei Chen,Bin Hu

Due to the high selectivity and stability, molecularly imprinted polymers (MIPs) have been successfully applied in stir bar sorptive extraction (SBSE) as a special coating to improve the selective extraction capability for target analytes. However, traditional MIPs usually suffer from incompatibility in aqueous media and low adsorption capacity, which limit the application of MIP coated stir bar in aqueous samples. To solve these problems, a water-compatible graphene oxides (GO)/MIP composite coated stir bar was prepared in this work by in situ polymerization. The prepared water-compatible GO/MIP coated stir bar presented good mechanical strength and chemical stability, and its recognition ability in aqueous samples was improved due to the polymerization of MIP in water environment, the adsorption capacity for target analytes was also increased by the addition of GO in MIP pre-polymer solution. Based on it, a method of water-compatible GO/MIP coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detector (HPLV-UV) was proposed for the analysis of propranolol (PRO) in aqueous solution. The influencing factors of SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-UV method was evaluated under the optimized conditions. The limit of detection (LOD) of the proposed method for PRO was about 0.37   μg   L −1 , and the enrichment factor (EF) was 59.7-fold (theoretical EF was 100-fold). The reproducibility was also investigated at concentrations of 5   μg   L −1 and the relative standard deviation (RSD) was found to be 7.3% (n   =   7). The proposed method of GO/MIP coating-SBSE-HPLC-UV was successfully applied for the assay of the interested PRO drug in urine samples, and further extended to the investigation of the excretion of the drugs by monitoring the variation of the concentration of PRO in urine within 10   h after drug-taking.

研究领域: 分析化学 · 药物分析 · 环境科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2014 · IF 4.258

Development of dual-templates molecularly imprinted stir bar sorptive extraction and its application for the analysis of environmental estrogens in water and plastic samples

Zhigang Xu,Zailei Yang,Zhimin Liu

In this study, a novel dual-template molecularly imprinted polymer (MIP)-coated stir bar was prepared and coupled with high-performance liquid chromatography (HPLC) for the analysis of environmental estrogens in complex samples. Dual-template MIP coating was homogeneous and porous with an average thickness of 5   μm. Moreover, it could be used for at least 50 times and be kept for at least 12 months in a dryer without any damage. The MIP-coated stir bar showed excellent selectivity to bisphenols and steroids. The method for the determination of bisphenols and steroids in complex samples via MIP-coated stir bar sorptive extraction coupled with HPLC was developed. The method was successfully applied in the analysis of five estrogens in lake and river water samples with recoveries of 71.2– 96.4% and 62.8–98.0%, respectively. The method was also successfully applied to the analysis of five estrogens in three plastic samples with recoveries of 67.7–99.1%, 68.8–99.9%, and 74.8–101.8%. The limit of quantitation was 1.0–5.0   μg/L. The proposed method is suitable for the simultaneous determination of multiple trace environmental estrogens in water and plastic samples.

CAS / MDL: 140-66-9 98-54-4
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
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2019 ·Vol. 411 ·期 10 ·2239-2248 · IF 3.286

Magnetic stir cake sorptive extraction of trace tetracycline antibiotics in food samples: preparation of metal–organic framework-embedded polyHIPE monolithic composites, validation and application

Du Fuyou,Sun Lingshun,Tan Wei,Wei Zongyu,Nie Honggang,Huang Zhujun,Ruan Guihua,Li Jianping

In this work, a novel Fe 3 O 4 @Cu 3 (btc) 2 -embedded polymerized high internal phase emulsion (Fe 3 O 4 @HKUST-1-polyHIPE) monolithic cake was synthesized, characterized and used as an adsorbent in the magnetic stir cake sorptive extraction (MSCSE) and determination of tetracycline antibiotics (TCs) in food samples by a combination of with high-performance liquid chromatography–fluorescence detection (HPLC-FLD). The prepared Fe 3 O 4 @HKUST-1-polyHIPE monolithic composites displayed a strong extraction ability and high column capacity due to enhanced interactions such as π–π interactions, hydrogen bonding, and electrostatic interactions. The extraction and desorption conditions were evaluated, and the calibration curves of four spiked TCs were linear ( R 2  ≥ 0.9991) in the range from 20 to 800 ng mL −1 for milk and egg samples, and 20 to 800 ng g −1 for chicken muscle and kidney samples. The limits of detection and the limits of quantification of the four TCs by using the proposed MSCSE-HPLC-FLD method were in the range of 1.9–4.6 and 5.5–13.9 ng mL −1 for milk and egg samples, and 1.8–3.7 and 5.3–13.0 ng g −1 for chicken muscle and kidney samples, respectively. The recoveries of the target TCs from spiked food samples were in the range from 86.6 to 110.7% with relative standard deviations lower than 7.0%. The proposed method was successfully applied for the determination of these four TCs in milk, egg, chicken muscle, and kidney samples.

研究领域: 分析化学 · 环境科学 · 食品安全
✓ 已验证 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY A · 2025 · IF 4

3D Printed Clear Resin Stir Bar Sorptive Extraction Coupled with High Performance Liquid Chromatography for Trace Chlorophenols Analysis in Environmental Water Samples

Ning Zhu,Zhichen Liu,Qiulin Zhang,Man He,Beibei Chen,Bin Hu

3D printing is an additive manufacturing technology based on digital model files. 3D printing has become a popular manufacturing tool in various fields. Stereolithography offers a series of advantages compared to its counterparts, such as smooth prints, appropriate resolution in all the axes, acceptable organic solvent compatibility and sufficient tightness to the flowing of solutions/solvents at moderate/high pressure. Thus, this work used stereolithography and clear resin (polymethyl methacrylate resin and epoxy resin) to prepare stir bars’ coatings, which reduced the size of the fabricated stir bar (1 mm) and no swelling property in organic solvents. In this work, three types of structures were designed as the coatings of stir bars, which were solid, discal, and lattice coatings with equal mass (0.13 g). Because of the largest surface area, lattice coatings were chosen to be make clear resin stir bars. The clear resin stir bars were used for stir bar sorptive extraction and combined with high performance liquid chromatography to develop a new method, which was successfully applied to detect four chlorophenols in environmental water samples. Compared with the previous work using melt deposition modeling 3D printing, this work could print hollow structures with higher precision. The stir bars could have higher rotational speed (700 rpm vs 350 rpm), smaller desorption volume (500 μL vs 2 mL), and shorter extraction time (60 min vs 90 min). The stir bars also had excellent mechanical performance and long lifetimes of up to 160 times. LODs of this method were between 0.30 μg/L (2-CP) and 0.97 μg/L (2,4,6-TCP) (S/N=3), which were below the concentration limits of surface water samples. Relative standard deviations of the stir bars were 1.4-3.9% (n=7, c=10 μg/L).

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
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